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At least 19 records

Environmental Stress Testing of the Single Sample Cylinder: A Proven Consensus Standard for Internal Gas Analysis (IGA) or Residual Gas Analysis (RGA)

In August 2008, Schuessler Consulting was contracted by NASA GSFC in support of the NASA Electronic Parts and Packaging (NEPP) program to perform two separate studies on moisture laden air in a stainless steel cylinder that had been designed to become a consensus standard for Test Method 1018. This Test Method was originally released for hybrids under Mil. Std. 883 but was quickly utilized on other microelectronic devices under the auspice of Mil. Std. 750. The cylinder had subsequently been fabricated for the 750 community. It was back-filled with moist air and subsequently analyzed over a period of time under a previous NASA contract. It had been shown that moisture in the 4000 - 5000 ppm range could be analyzed rather precisely with a mass spectrometer, commonly referred to as a Residual Gas Analyzer (RGA). The scope of this study was to ascertain if the composition and precision varied as a function of thermal shock at sub-zero temperatures and whether there was consensus when the standard was submitted to other RGA units. It was demonstrated and published that the consensus standard would yield precise RGA data for moisture within +/- 1% when optimized for a given RGA unit. It has been subsequently shown in this study at Oneida Research Services, that sub-zero storage did not affect that precision when a well-defined protocol for the analysis was followed. The consensus standard was taken to a second facility for analysis where it was found that moisture adsorption on the transfer lines caused precision to drop to +/- 12%. The Single Sample Cylinder (SSC) is a one liter stainless steel cylinder with associated sampling valves and has considerable weight and volume. But this considerable size allows for approximately 300 gas samples of the same composition to be delivered to any RGA unit. Lastly, a smaller cylinder, approximately 75 cc, of a second consensus standard was fabricated and tested with a different mix of fixed gases where moisture was kept in the 100 ppm range. This second standard has the potential of providing 30 gaseous samples and can be readily shipped to any analytical facility that desires to generate comparison RGA data. A series of comparison residual gas analyses was performed at the Honeywell Federal Manufacturing & Technologies facility in the National Nuclear Facility Administration s plant in Kansas City to complete this project. It was shown that improvements in the precision of a given RGA unit can be done by controlling the cycle time for each analysis and increasing analysis temperatures to minimize moisture adsorption. It was also found that a "one time event" in the subzero storage of the large SSC did not effect the units ability to continuously supply precise samples of the same chemistry, however the "event" caused a permanent +8% shift in the reported value of the moisture content. Lastly, a set of SSC RGA results was plotted on a common graph with DSCC "correlation study" RGA data. The result demonstrates the ability of the SSC to remove many of the individual variances that single, individual samples introduce. The consensus standards are now in storage at Oneida Research Services, one of the DSCC certified houses that does RGA to Military Standards, where they await future studies. The analytical data and the operational parameters of the instruments used are provided in the following discussion. Limitations and suggested means for improvement of both precision and accuracy are provided.

Schuessler, Philipp WH↗

AmeriFlux FLUXNET-1F US-RGA Arkansas Corn Farm

This is the AmeriFlux Management Project (AMP) created FLUXNET-1F version of the carbon flux data for the site US-RGA Arkansas Corn Farm. This is the FLUXNET version of the carbon flux data for the site US-RGA Arkansas Corn Farm produced by applying the standard ONEFlux (1F) software. Site Description - Commercially farmed corn-soy rotation in Arkansas County, Arkansas. Part of a multi-year, ground-truthing field study under the DOE ARPA-E SMARTFARM project.

Schuppenhauer, Michael R.↗

AmeriFlux US-RGA Arkansas Corn Farm

This is the AmeriFlux version of the carbon flux data for the site US-RGA Arkansas Corn Farm. Site Description - Commercially farmed corn-soy rotation in Arkansas County, Arkansas. Part of a multi-year, ground-truthing field study under the DOE ARPA-E SMARTFARM project.

Schuppenhauer, Michael R.↗

Understanding the Quadrupole Mass Filter and Testing a High-Resolution QMS RGA for ITER

A common type of residual gas analyzer is the quadrupole mass spectrometer. One of the main components within this instrument is a mass filter known as the quadrupole. It is responsible for the selective throughput of the ionized gas particles - by ascending mass number - prior to ion impacts on the analyzer (or detector) surface from which the ion current signal is generated for processing. However, the quadrupole is not fully described in relation to the electric field characteristics and the function as an ion mass separator. This paper describes the basic origins of the electrical design, the intricate assembly criteria, and performance of the quadrupole within the spectrometer. A specialized quadrupole mass spectrometer is part of a configuration for a diagnostic gas analyzer system planned for ITER, a fusion research machine. It has a verified capability, essential as a diagnostic criterion for this reactor project, to successfully deconvolute the mass signals of Helium-4 and deuterium (reactor fuel exhaust gases, separated by only 0.026 atomic mass units), down to a relative three-percent concentration of the former gas. The associated preliminary testing, performed at the Oak Ridge National Laboratory, is also addressed. Finally, one of the key parameters used to express gas concentration, the relative sensitivity factor, will be explained, including an evaluation of dependency on other variables.

Marcus, Chris [ORNL] (ORCID:0000000190139636)↗

Graphic Three-Axes Presentation of Residual Gas Analyzer Data

Residual gas analyzers (RGA) are commonly used to measure the composition of residual gases in thermal-vacuum test chambers. Measurements from RGA's are often used to identify and quantify outgassing contaminants from a test article during thermal-vacuum testing. RGA data is typically displayed as snapshots in time, showing instantaneous concentrations of ions from ionized residual gas molecules at different atomic masses. This ion concentration information can be interpreted to be representative of the composition of the residual gas in the chamber at the instant of analysis. Typically, test personnel are most interested in tracking the time history of changes in the composition of chamber residual gas to determine the relative cleanliness and the clean-up rate of the test article under vacuum. However, displays of instantaneous RGA data cannot provide test personnel with the preferred time history information. In order to gain an understanding of gas composition trends, a series of plots of individual data snapshots must be analyzed. This analysis is cumbersome and still does not provide a very satisfactory view of residual gas composition trends. A method was devised by the authors to present RCA data in a three-axis format, plotting Atomic Mass Unit (AMU), the Ionization Signal Response (ISR) as amps/torr as a function of AMU, and Time, to provide a clear graphic visualization of trends of changes in ISR with respect to time and AMU (representative of residual gas composition). This graphic visualization method provides a valuable analytical tool to interpret test article outgassing rates during thermal vacuum tests. Raw RGA data was extracted from a series of delimited ASCII files and then converted to a data array in a spreadsheet. Consequently, using the 3-D plotting functionality provided by the spreadsheet program, 3-D plots were produced. After devising the data format conversion process, the authors began developing a program to provide real-time 3-D plotting of RGA data. The intent of this program is to automate the RGA data acquisition process and to generate up-to-the-minute time history 3-D displays of stored RGA data (development of this program was not complete at the time of this writing). This paper provides a brief description of the data format conversion process and presents results from a recent test to illustrate the usefulness of this 3-D RGA data plotting technique.

Johnson, Kenneth R.↗

Automating a residual gas analyzer

A residual gas analyzer (RGA), a device for measuring the amounts and species of various gases present in a vacuum system is discussed. In a recent update of the RGA, it was shown that the use of microprocessors could revolutionize data acquisition and data reduction. This revolution is exemplified by the Inficon 1Q200 RGA which was selected to meet the needs of this update. The Inficon RGA and the Zilog microcomputer were interfaced in order the receive and format the digital data from the RGA. This automated approach is discussed in detail.

Petrie, W. F.↗

Reflection Grating Array Associated with the Reflection Grating Spectrometer Developed by the Space Research Organization of the Netherlands for the X-ray Multi-Mirror Mission (XMM)

The University of California, Berkeley (UCB) served as the Principal Investigator institution for the United States participation in the development of the Reflection Grating Spectrometer (RGS) which included the design, development, fabrication, and testing of the Reflection Grating Assembly (RGA). UCB was assisted in this role by the Lawrence Livermore National Laboratory and Columbia University who provided the primary facilities, materials, services and personnel necessary to complete the development. UC Berkeley's Dr. Steven Kahn provided the technical and scientific oversight for the design. development and testing of the RGA units by monitoring the performance of the units at various stages in their development. Dr. Kahn was also the primary contact with the Space Research Organization of the Netherlands (SRON) and represented the RGA development at all SRON and European Space Agency (ESA) reviews of the RGA status. In accordance with the contract, the team designed and developed novel optical technology to meet the unique requirements of the RGS. The ESA XMM-Newton Mission carries two identical Reflection Grating Spectrometers (RGS) behind two of its three nested sets of Wolter I type mirrors. The instrument allows high-resolution measurements in the soft X-ray range (6 to 38 angstroms or 2.1 to 0.3 keV) with a maximum effective area of about 140 sq cm at 15 angstroms. Its design is optimized for the detection of the K-shell transitions of carbon, nitrogen, oxygen, neon, magnesium, and silicon. as well as the L shell transitions of iron. The RGA itself consists of two units. A structure for each unit was designed to hold up to 220 gratings. In its final configuration, one unit holds 182 gratings and the second hold 181 gratings.

Kahn, Steven M.↗

Residual Gas Analyzer Calibration

A technique which employs known gas mixtures to calibrate the residual gas analyzer (RGA) is described. The mass spectra from the RGA are recorded for each gas mixture. This mass spectra data and the mixture composition data each form a matrix. From the two matrices the calibration matrix may be computed. The matrix mathematics requires the number of calibration gas mixtures be equal to or greater than the number of gases included in the calibration. This technique was evaluated using a mathematical model of an RGA to generate the mass spectra. This model included shot noise errors in the mass spectra. Errors in the gas concentrations were also included in the valuation. The effects of these errors was studied by varying their magnitudes and comparing the resulting calibrations. Several methods of evaluating an actual calibration are presented. The effects of the number of gases in then, the composition of the calibration mixture, and the number of mixtures used are discussed.

R H Lilienkamp↗

Automated measurement of respiratory gas exchange by an inert gas dilution technique

A respiratory gas analyzer (RGA) has been developed wherein a mass spectrometer is the sole transducer required for measurement of respiratory gas exchange. The mass spectrometer maintains all signals in absolute phase relationships, precluding the need to synchronize flow and gas composition as required in other systems. The RGA system was evaluated by comparison with the Douglas bag technique. The RGA system established the feasibility of the inert gas dilution method for measuring breath-by-breath respiratory gas exchange. This breath-by-breath analytical capability permits detailed study of transient respiratory responses to exercise.

Sawin, C. F.↗

Hubble space telescope component qualification utilizing a residual gas analyzer

An approach is described for integrating an automated residual gas analyzer (RGA) into the thermal vacuum outgas process. The RGA has the capability of detailed analysis over a 200 amu range with monitoring of each peak as the test progresses. The NASA criterion of either a 50% reduction of each peak over 44 amu or less than an 0.1% amplitude of the 28 amu base peak for all amu's above 44 amu is satisfied. A computer sorts, reports which peaks do not satisfy the criterion, and reports test completion. The computer plots amplitudes of all the peaks from 1 amu through 200 amu for each scan. This RGA real time approach is unique in that it provides sufficient detail to highlight a problem as it occurs. By comparison, a quartz crystal microbalance (QCM) or a thermoelectric quartz crystal microbalance (TQCM) indicates to the operator when changes occur, but not what has happened. Optical witness samples indicate whether a test was satisfactory within a few days after the test was completed.

Westfall, A. H.↗

Material Outgassing, Identification and Deposition, MOLIDEP System

The outgassing tests are performed employing a modified vacuum operated Cahn analytical microbalance, identified as the MOLIDEP system. The test measures under high vacuum, the time varying Molecular mass loss of a material sample held at a chosen temperature; it Identifies the outgassing molecular components using an inline SRS 300 amu Residual Gas Analyzer (RGA) and employs a temperature controlled 10 MHz Quartz Crystal Microbalance (QCM) to measure the condensable DEPosits. Both the QCM and the RGA intercept within the conductive passage the outgassing products being evacuated by a turbomolecular pump. The continuous measurements of the mass loss, the rate of loss, the sample temperature, the rate of temperature change, the QCM temperature and the QCM recorded condensable deposits or rate of deposits are saved to an Excel spreadsheet. A separate computer controls the RGA.

Scialdone, John J.↗

Graphic Three-Axes Presentation of Residual Gas Analyser Data

Residual gas analyzers (RGA) are commonly used to measure the composition of residual gases in thermal-vacuum test chambers. Measurements from RGAs are often used to identify and quantify outgassing contaminants from a test article during thermal-vacuum testing. RGA data is typically displayed as snapshots in time, showing instantaneous concentrations of ions from ionized residual gas molecules at different atomic masses. A method was devised by the authors to present RGA data in a three-axis format, plotting atomic mass unit (AMU), ion concentration as a function of AMU, and time, to provide a clear graphic visualization ot trends in gas concentration changes and to initiate a valuable analytical tool to interpret test article outgassing rates during thermal-vacuum testing.

data analysis↗

Developing Mass Spectrometry for Water Quantitation and Volatiles Analysis from In-Situ Regolith

With a revived focus to create a sustainable hu-man presence on the moon, and in preparation for future Mars exploration, it is imperative that all resources are utilized to their fullest potential [1]. In-Situ Resource Utilization (ISRU) will be critical for future mission success as it would enable in-dependent operation of missions while reducing the dependence on the complex supply chain created between the Earth, the moon and Mars. One of the most critical resources that has been identified for ISRU on the lunar surface is water [2]. Water is a versatile resource that can be used in various space operations, such as ra-diation shielding and conversion to oxygen (O2) for propellant [3,4]. One of the most water rich resources is thought to be within the regolith lo-cated in the permanently shadowed regions (PSR) of the Moon; several upcoming missions, such as PRIME-1 and VIPER, are already sched-uled to confirm this hypothesis [5,6]. However, there are currently no missions planned to quanti-fy the abudance of water at these regions. The quantity of water contained in the ice will inform and help the development of future ISRU plants and operation. Water and other volatile gases can be detect-ed upon controlled heating of icy lunar regolith for an accurate quantification of water. This method is similar to thermogravimetric analysis, which was used to analyze Apollo lunar regolith sam-ples. However, losses via sublimation/evaporation or contamination may have occurred with the samples due to the transit and exposure to the terrestrial environment. Furthermore, water would not be expected for these samples since they were not collected from a PSR. Thus, for more accurate results, icy lunar regolith should be ana-lyzed in situ to provide the most representative composition of both water and other volatile gas-es. The Light Water Analysis and Volatile Extract (LightWAVE) project aims to address this knowledge gap. A system has been developed to collect, heat and analyze evolved gases from lu-nar regolith on the lunar surface. The gases will be analyzed by a modified commercial off the shelf (COTS) residual gas analyzer (RGA) quad-rupole mass spectrometer. Evolved gases from heated regolith samples can be identified by the observed mass-to-charge (m/z) ratios, and the peak intensities correlate to the abundances of the observed gases for quantitation. Therefore, our group is developing a calibration methodology utilizing a COTS RGA to quantitate water from in-situ regolith samples on the lunar surface. The partial pressure of water and ideal gas law will be used to quantify the total water evolved from a regolith sample. Here we present our methodol-ogy for the design and calibration for water quan-titation using a COTS RGA.

Nilab Azim↗

Green_Revolution_genes_in_Populus

This dataset contains the stem RNA-seq data of Populus tremula x P. alba genotypes of RGA triple knockout. Populus genotypes in this study includes the empty vector control (EV, Cas9-19) and three independent RGA triple mutants, 267-17 (RGAX4KO_17), 267-2

09 BIOMASS FUELS↗

Extreme Ultraviolet and Beyond Extreme Ultraviolet Lithography Using Amorphous Zeolitic Imidazolate Resists Deposited by Atomic/Molecular Layer Deposition

Amorphous zinc-imidazolate (aZnMIm) resists show potential to meet the demands for next-generation high-numerical aperture (high-NA) metal-containing extreme ultraviolet (EUV) resist materials, given their ease of deposition by atomic/molecular layer deposition (ALD/MLD) at thicknesses of 20 nm and below. Here, this study demonstrates that aZnMIm thin films, previously identified as high-resolution electron beam resists, can also function as negative-tone EUV photoresists. Water development achieves high sensitivity (5 mJ/cm 2 ) but leaves significant residue, while acetic acid development results in poor contrast. A hybrid approach─water followed by acetic acid─enables residue-free development with a sensitivity of 181 mJ/cm 2 . Dry development using 1,1,1,5,5,5-hexafluoroacetylacetone (hfacH) is also possible but shows lower sensitivity (375 mJ/cm 2 ) compared to wet development methods. EUV photoelectron spectroscopy (PES), reflectometry/EUV absorption, total electron yield (TEY), residual gas analysis (RGA), and time-of-flight secondary ion mass spectrometry (TOF-SIMS) were used to investigate the effects of EUV irradiation on aZnMIm resists. Reflectometry experiments reveal an aZnMIm EUV absorption coefficient of 6.2 μm –1 , while PES and TEY analyses show that, compared to poly(4-hydroxystyrene) (PHS), a polymer-based reference resist, aZnMIm emits more primary and secondary electrons but generates fewer slow electrons relative to its primary electron emission; its total electron yield is similar to that of poly(methyl methacrylate) (PMMA) resists. When exposed to EUV, aZnMIm predominantly outgasses H 2 , as determined by RGA. TOF-SIMS measurements demonstrate that high-dose EUV exposure only partially fragments the 2-methylimidazole (2MIm) organic linkers, unlike high-dose electron beam exposure, which is known to completely degrade them. Additionally, aZnMIm resists show promise for potential beyond EUV lithography (BEUVL) due to the presence of Zn, which provides higher sensitivity at a wavelength of 6.7 nm compared to other metal ions, such as Sn, that are currently used in the best-performing EUV metal–organic resists. TEY measurements demonstrate that aZnMIm emits nearly twice as many electrons as PHS at 6.7 nm. The BEUV TEY of aZnMIm also surpasses that of PMMA, poly(pentafluorostyrene), and poly(4-iodostyrene), with the latter two being known for their high EUV TEYs. This work provides insight into zeolitic imidazolate framework (ZIF)-based EUV and BEUV resists and highlights their potential for both wet and dry development.

lithography↗

In situ effective pumping speed measurements as a tool for non-evaporable getter activation and saturation monitoring

We have developed method of in situ effective pumping speed measurements based on injecting finite gas pulse into a vacuum volume and subsequent recording of pressure response using a Residual Gas Analyzer (RGA). The pressure burst caused by injected gas pulse falls exponentially in time and the exponential coefficient of such pressure decay is proportional to total effective pumping speed of all vacuum pumps acting on vacuum chamber volume. The effective pumping speed can be extracted from the dependence of injected gas species pressure vs time recorded by an RGA. Non-Evaporable Getters (NEGs) are widely used in multiple ultra and extremely high vacuum devices and applications during the last several decades. Areas of NEG applications were recently expanded into vacuum devices with relatively high-pressure levels (up to 10 -7 Torr) by the invention of high capacity ZAO NEG which can be operated at elevated temperatures. The intrinsic property of all NEG-based vacuum pumps is the reduction of their pumping speed, called “NEG saturation”, after an extended period of operation. Typical time interval for such process can span from about a month and up to a few years depending on NEG type, vacuum level of NEG pump operation, and residual gas content. After that, the NEG pump will require a re-activation cycle to restore its pumping speed close to the initial value. For many applications it is difficult to realize what is the current pumping speed of NEG pump is and when the pump should be re-activated. A method for in situ effective pumping speed measurements developed in this study can be used as a tool for NEG-based pump activation and saturation monitoring. Application of such an approach to monitor pumping status of NEG pumps was utilized and will be continually used at Extended EBIS which was recently developed and commissioned for Relativistic Heavy Ion Collider (RHIC) and future Electron Ion Collider (EIC). The results obtained during commissioning are presented and discussed.

43 PARTICLE ACCELERATORS↗