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Inficon Transpector MPH Mass Spectrometer Random Vibration Test Report

The purpose of this test report is to summarize results from the vibration testing of the INFICON Transpector MPH100M model Mass Spectrometer. It also identifies requirements satisfied, and procedures used in the test. As a payload of Resource Prospector, it is necessary to determine the survivability of the mass spectrometer to proto-qualification level random vibration. Changes in sensitivity of the mass spectrometer can be interpreted as a change in alignment of the instrument. The results of this test will be used to determine any necessary design changes as the team moves forward with flight design.

Transpector↗

Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better detection via good peak separation with a longer run time is a better asset than moderate peak separation with a shorter run time. Even given that RESOLVE is highly interested in water and that mission timeline is of significant importance given the short seven-to-ten-day mission timeline, worse detection with an 8m column may lead to overlooking other substances existing on the moon that could advance planetary science. Thus, I recommend the 20m column. However, if mission timeline and water separation are deemed the highest priority, the 8m column should be selected due to its ability to separate water within a shorter run time than the 20m column.

Column↗

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.↗

Simple evaporation controller for thin-film deposition from a resistively heated boat

A simple, inexpensive circuit is described for switching the current through a resistively heated evaporation boat during thin-film deposition. The circuit uses a silicon-controlled rectifier (SCR) to switch the 0-15-A current in the primary of a 2-kV A step-down transformer that supplies the 0-200-A current to an evaporation boat. The circuit is controlled by a 0-10 V-dc signal similar to that furnished by an Inficon XTC deposition-rate controller. This circuit may be assembled from a handful of parts for a cost of about $400, nearly one-tenth the cost of similar commercial units. Minimum construction is required, since the circuit is built around an off-the-shelf, self-contained SCR unit.

Scofield, John H.↗

Evaluating Mass Analyzers as Candidates for Small, Portable, Rugged Single Point Mass Spectrometers for Analysis of Permanent Gases

For Space Shuttle launch safety, there is a need to monitor the concentration Of H2, He, O2, and Ar around the launch vehicle. Currently a large mass spectrometry system performs this task, using long transport lines to draw in samples. There is great interest in replacing this stationary system with several miniature, portable, rugged mass spectrometers which act as point sensors which can be placed at the sampling point. Five commercial and two non-commercial analyzers are evaluated. The five commercial systems include the Leybold Inficon XPR-2 linear quadrupole, the Stanford Research (SRS-100) linear quadrupole, the Ferran linear quadrupole array, the ThermoQuest Polaris-Q quadrupole ion trap, and the IonWerks Time-of-Flight (TOF). The non-commercial systems include a compact double focusing sector (CDFMS) developed at the University of Minnesota, and a quadrupole ion trap (UF-IT) developed at the University of Florida.

Arkin, C. Richard↗

Evaluating Mass Analyzers as Candidates for Small, Portable, Rugged Single Point Mass Spectrometers for Analysis of Permanent Gases

For Space Shuttle launch safety, there is a need to monitor the concentration of H2, He, O2 and Ar around the launch vehicle. Currently a large mass spectrometry system performs this task, using long transport lines to draw in samples. There is great interest in replacing this stationary system with several miniature, portable, rugged mass spectrometers which act as point sensors which can be placed at the sampling point. Five commercial and two non-commercial analyzers are evaluated. The five commercial systems include the Leybold Inficon XPR-2 linear quadrupole, the Stanford Research (SRS-100) linear quadrupole, the Ferran linear quadrupole array, the ThermoQuest Polaris-Q quadrupole ion trap, and the IonWerks Time-of-Flight (TOF). The non-commercial systems include a compact double focusing sector (CDFMS) developed at the University of Minnesota, and a quadrupole ion trap (UF-IT) developed at the University of Florida. The System Volume is determined by measuring the entire system volume including the mass analyzer, its associated electronics, the associated vacuum system, the high vacuum pump and rough pump. Also measured are any ion gauge controllers or other required equipment. Computers are not included. Scan Time is the time required for one scan to be acquired and the data to be transferred. It is determined by measuring the time required acquiring a known number of scans and dividing by said number of scans. Limit of Detection is determined first by performing a zero-span calibration (using a 10-point data set). Then the limit of detection (LOD) is defined as 3 times the standard deviation of the zero data set. (An LOD of 10 ppm or less is considered acceptable.)

Arkin, C. Richard↗

Evaluation of Small Mass Spectrometer Systems

Various mass analyzer systems were evaluated. Several systems show promise, including the Stanford Research Systems RGA-100, Inficon XPR-2, the University of Florida's Ion Trap, and the Compact Double Focus Mass Spectrometer. Areas that need improvement are the response time, recovery time, system volume, and system weight. Future work will investigate techniques to improve systems and will evaluate engineering challenges.

Arkin, C. Richard↗

Documenting Surface and Sub-surface Volatiles While Drilling in Frozen Lunar Simulant

NASA's Resource Prospector (RP) mission is intended to characterize the three-dimensional nature of volatiles in lunar polar regions and permanently shadowed regions. RP is slated to carry two instruments for prospecting purposes. These include the Neutron Spectrometer System (NSS) and Near-Infrared Volatile Spectrometer System (NIRVSS). A Honybee Robotics drill (HRD) is intended to sample to depths of 1 m, and deliver a sample to a crucible that is processed by the Oxygen Volatile Extraction Node (OVEN) where the soil is heated and evolved gas is delivered to the gas chromatograph / mass spectrometer of the Lunar Advanced Volatile Analysis system (LAVA). For several years, tests of various sub-systems have been undertaken in a large cryo-vacuum chamber facility (VF-13) located at Glenn Research Center. In these tests a large tube (1.2 m high x 25.4 cm diameter) is filled with lunar simulant, NU-LHT-3M, prepared with known abundances of water. There are thermo-couples embedded at different depths, and also across the surface of the soil tube. The soil tube is placed in the chamber and cooled with LN2 as the pressure is reduced to approx.5-6x10(exp -6) Torr. Here we discuss May 2016 tests where two soil tubes were prepared and placed in the chamber. Also located in the chamber were 5 crucibles, an Inficon mass spectrometer, and a trolly permitting x-y translation, where the HRD and NIRVSS, were mounted. The shroud surrounding the soil tube was held at different temperatures for each tube to simulate a warm and cold lunar environment.

Oxygen Volatile Extraction Node↗

GEER Status Update

History: The Glenn Extreme Environments Rig (GEER) first became operational in the early part of 2015. Since that time GEER has completed a number of scientific tests and has undergone improvements in the chemical delivery system and analytics following a year of operations experience. Recent Updates: In June 2016, the GEER process system was rebuilt to provide a more robust system, higher accuracy and new capabilities. New insulation was installed on the exterior of the pressure vessel and gas lines. The newly revamped GEER plumbing system can provide extremely precise custom gas mixtures using any gas desired by the investigator in any combination. GEER can heat the resulting mixture up to 500 deg C and 1500 psia. The 304 stainless steel vessel walls were polished to reduce corrosion rate and reduce unwanted chemical reactions. The process lines were replaced with high purity Sulfinert coated tubing. The GEER team added the ability to individually boost specialty gases to GEER thus allowing operators to make very precise changes to the gas chemistry inside of GEER during a test while at high temperature and pressure. High accuracy mass flow meters were added to further improve gas mixing accuracy and precision. An in-line, integrated Inficon MicroGC Fusion was added for real time gas analysis along with a high purity gas sampling system, providing fully automated, real time analysis of the gas chemistry inside of GEER in minutes. This complements a co-located mass spectrometer and both are used for regular monitoring of the vessel chemistry. All internal vessel components were replaced with polished 304SS equivalents. Hot vent down capability was increased. Finally, an automated liquid injection system was added and is rated for max vessel operating conditions of (1500 psia, 500 C). Recent Results and Publications: In May 2016, GEER completed a test that exposed high temperature electronics to Venus surface conditions for 21.5 days. This demonstrated the potential for operating robotic spacecraft in the Venus environment without the need for thermal or environmental protection. Results from this test were published in December 2016 and received national media attention. In April 2017 GEER implemented an 80 day test at Venus surface conditions to simulate chemical weathering of expected Venus minerals. This test supported a ROSES award to a team led by Prof. Ralph Harvey of Case Western Reserve University. The test concluded in July 2017 and nearly doubled previous operation record of 42 days at Venus surface conditions. Preliminary results of these and previous experiments were presented at the recent Venus Modeling Workshop. In June 2017, NASA TM2017-219437 "Chemical and Microstructural Changes in Metallic and Ceramic Materials Exposed to Venusian Surface Conditions" was published. This report provides an extensive and valuable resource detailing the behavior of a variety of engineering materials at Venus surface conditions. Community Involvement: An external science advisory panel has been formed.

Kremic, Tibor↗

Spectral Monitoring of Volatiles During Drilling into Frozen Lunar Simulant

NASA's Resource Prospector (RP) project intends to characterize the 3D distribution of volatiles in permanently shadowed regions at the lunar poles. One RP remote sensing instrument is a near-infrared spectrometer with an associated camera and radiometer, called the Near-InfraRed Volatile Spectrometer System (NIRVSS). In May 2016, NIRVSS, a Honeybee Robotics drill, and an Inficon mass spectrometer were placed in a vacuum chamber at Glenn Research Center. Also inside was a tube (1.2 m high x 25 cm diameter) filled with lunar simulant NU-LHT-3M, initially doped with a homogeneous water abundance of ~5%, chilled to cryogenic temperatures and exposed to a vacuum (~10e-6 Torr). During drilling, the NIRVSS instruments observed the cuttings pile as subsurface materials were emplaced on the surface. Spectral features associated with water ice, near 2000 and 3000 nm, were measured by the spectrometer during drilling. The spectral data documents development of a desiccated soil layer in the tube down to ~25-30 cm (confirmed by post-test soil analyses), formed during the initial pump down to vacuum. Drilling occurred in 10 cm segments, with the drill stem extracted and flutes brushed after each 10 cm depth. One exception to this was the 40 cm depth segment where the soil was delivered to a sample capture mechanism, and sealed for post-test analyses. To ~30 cm depth the greatest 2000 and 3000 nm signatures were associated with brushing of the drill flutes above the surface. At depths >40 cm the strongest ice signatures were associated with the drill clearing soil from the existing hole, or beginning to encounter new material. For these greater depths, brushing the flutes after extraction produced much weaker ice signatures than for shallower depths. This suggests that the soil may remain trapped in the exit funnel and is not emplaced on the surface. After each event creating strong ice signatures, these signatures decreased to near background levels in 5 minutes or less, due to surface exposure to vacuum.

lunar poles↗