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This paper presents a summary of the planetary protection technology development efforts currently being conducted at the Jet Propulsion Laboratory (JPL). This is a multidisciplinary effort involving JPL and NASA expertise in microbiology, material science, and analytical chemistry, in conjunction with outside, industrial academic collaborators.
The Spacecraft Water Impurity Monitor (SWIM) is a joint collaboration to develop an instrument platform that will perform in-flight measurements and deliver a more complete picture of water quality to decision makers. Eventually, missions to the moon, Mars, and beyond will be equipped with analytical capabilities equaling those found in terrestrial labs. Based on what we know about current and future spacecraft environments, SWIM will seek to provide enhanced analytical capability that enables NASA to confidently send astronauts on distant missions without the possibility of returned water samples. This paper discusses the challenges presented by exploration requirements and the research and development progress toward the goal of a total water analysis system. For organic analysis, one of the analysis technologies that the SWIM team have been developing is a liquid-injection gas chromatograph mass spectrometer system; these systems are the workhorses of analytical chemistry laboratories world-wide. For inorganic analysis, the team is exploring a number of technologies ranging from traditional liquid chromatography technologies (e.g. ion chromatography, capillary electrophoresis) to flight-heritage technology such as ion-specific electrodes.
The Spacecraft Water Impurity Monitor (SWIM) is a joint collaboration to develop an instrument platform that will perform in-flight measurements and deliver a more complete picture of water quality to decision makers. For exploration missions, returned water samples will not be an option, so spacecraft and habitats will need to be equipped with advanced water monitoring capabilities. Eventually, missions to the moon, Mars, and beyond should be equipped with analytical capabilities roughly analogous to those found in terrestrial labs. Based on what we know about current and future spacecraft environments, SWIM will seek to provide enhanced analytical capability that enables NASA to confidently send astronauts on distant missions without the possibility of returned water samples. The SWIM architecture can be broken down in an Organic Water Module (OWM) and an Inorganic Water Module (IWM), independent of each other but can be flown together if desired; an integrated system may share some commonality, e.g., single sample injection, sampling consumables, waste, etc. Each of these main modules can be broken down further into separation (if required) and detection modules. And, each separation module can be paired with one or more detection module depending on mission, spacecraft, customer needs, and size/mass/power constraints. This paper discusses the research and development progress toward the goal of a total water analysis system. For OWM, one of the analysis technologies that the SWIM team have been developing is a liquid-injection gas chromatograph mass spectrometer system; these systems are the workhorses of analytical chemistry laboratories world-wide. For IWM, the team is exploring a number of technologies ranging from traditional liquid chromatography technologies (e.g. ion chromatography, capillary electrophoresis) to flight-heritage technology such as ion-specific electrodes.
The Spacecraft Water Impurity Monitor (SWIM) is a joint collaboration to develop an instrument platform that will perform in-flight measurements and deliver a more complete picture of water quality to decision makers. For exploration missions, returned water samples will not be an option, so spacecraft and habitats will need to be equipped with advanced water monitoring capabilities. Eventually, missions to the moon, Mars, and beyond should be equipped with analytical capabilities roughly analogous to those found in terrestrial labs. Based on what we know about current and future spacecraft environments, SWIM will seek to provide enhanced analytical capability that enables NASA to confidently send astronauts on distant missions without the possibility of returned water samples. The SWIM architecture can be broken down in an Organic Water Module (OWM) and an Inorganic Water Module (IWM), independent of each other but can be flown together if desired; an integrated system may share some commonality, e.g., single sample injection, sampling consumables, waste, etc. Each of these main modules can be broken down further into separation (if required) and detection modules. And, each separation module can be paired with one or more detection module depending on mission, spacecraft, customer needs, and size/mass/power constraints. This paper discusses the research and development progress toward the goal of a total water analysis system. For OWM, one of the analysis technologies that the SWIM team have been developing is a liquid-injection gas chromatograph mass spectrometer system; these systems are the workhorses of analytical chemistry laboratories world-wide. For IWM, the team is exploring a number of technologies ranging from traditional liquid chromatography technologies (e.g. ion chromatography, capillary electrophoresis) to flight-heritage technology such as ion-specific electrodes.
The Spacecraft Water Impurity Monitor (SWIM) is a joint collaboration to develop an instrument platform that will perform in-flight measurements and deliver a more complete picture of water quality to decision makers. For exploration missions, returned water samples will not be an option, so spacecraft and habitats will need to be equipped with advanced water monitoring capabilities. Eventually, missions to the moon, Mars, and beyond should be equipped with analytical capabilities roughly analogous to those found in terrestrial labs. Based on what we know about current and future spacecraft environments, SWIM will seek to provide enhanced analytical capability that enables NASA to confidently send astronauts on distant missions without the possibility of returned water samples. The SWIM architecture can be broken down in an Organic Water Module (OWM) and an Inorganic Water Module (IWM), independent of each other but can be flown together if desired; an integrated system may share some commonality, e.g., single sample injection, sampling consumables, waste, etc. Each of these main modules can be broken down further into separation (if required) and detection modules. And, each separation module can be paired with one or more detection module depending on mission, spacecraft, customer needs, and size/mass/power constraints. This paper discusses the research and development progress toward the goal of a total water analysis system. For OWM, one of the analysis technologies that the SWIM team have been developing is a liquid-injection gas chromatograph mass spectrometer system; these systems are the workhorses of analytical chemistry laboratories world-wide. For IWM, the team is exploring a number of technologies ranging from traditional liquid chromatography technologies (e.g. ion chromatography, capillary electrophoresis) to flight-heritage technology such as ion-specific electrodes.
The Spacecraft Water Impurity Monitor (SWIM) is a joint collaboration to develop an instrument platform that will perform in-flight measurements and deliver a more complete picture of water quality to decision makers. For exploration missions, returned water samples will not be an option, so spacecraft and habitats will need to be equipped with advanced water monitoring capabilities. Eventually, missions to the moon, Mars, and beyond should be equipped with analytical capabilities roughly analogous to those found in terrestrial labs. Based on what we know about current and future spacecraft environments, SWIM will seek to provide enhanced analytical capability that enables NASA to confidently send astronauts on distant missions without the possibility of returned water samples. The SWIM architecture can be broken down in an Organic Water Module (OWM) and an Inorganic Water Module (IWM), independent of each other but can be flown together if desired; an integrated system may share some commonality, e.g., single sample injection, sampling consumables, waste, etc. Each of these main modules can be broken down further into separation (if required) and detection modules. And, each separation module can be paired with one or more detection module depending on mission, spacecraft, customer needs, and size/mass/power constraints. This paper discusses the research and development progress toward the goal of a total water analysis system. For OWM, one of the analysis technologies that the SWIM team have been developing is a liquid-injection gas chromatograph mass spectrometer system; these systems are the workhorses of analytical chemistry laboratories world-wide. For IWM, the team is exploring a number of technologies ranging from traditional liquid chromatography technologies (e.g. ion chromatography, capillary electrophoresis) to flight-heritage technology such as ion-specific electrodes.
A "coffee-break" presentation on REE characterization invited to demonstrate an aspect of energy research at NETL involving Analytical Chemistry and Spectroscopy
Scanning confocal Raman microspectroscopy (RMS) was used to analyze thin sections for inorganic mineral content and for evaluation of organic material (OM). Thin sections were selected from a stratigraphic test well core in the Powder River Basin, Wyoming under the Wyoming CarbonSAFE project. The well was analyzed with a variety of rock and fluid characterization techniques to determine the feasibility of a commercial-scale CO2 storage site. RMS complements other analyses, including traditional petrography, SEM, porosity and permeability, and XRD For this aspect of the study, RMS is especially important in the evaluation of OM in sealing lithologies. At prospective geologic CO2 storage sites, it is imperative to assess the unconventional oil and gas potential of seals to ensure that any future development would not compromise the integrity of the seals. Whole-slide mineralogical surveys were performed on thin sections from various shale and sandstone formations. Surveys were analyzed with Direct Classical Least Squares to identify and quantify minerals. The location and concentration of minerals was color-coded and overlaid on optical images for visualization of the distribution of minerals. Dense hyperspectral Raman mapping of OM was performed on five thin sections. Eleven spectral parameters diagnostic of organic type and thermal maturity were used to train a Partial Least Squares (PLS) calibration against a set of artificially matured samples spanning the pre- to mid-oil window. The PLS was applied to the study set and a post-mature set. Additionally, the PLS was applied to each point in hyperspectral maps for visualization of trends in maturity across sample sets and discrimination of organic matter types within a given map. In inorganic surveys on thin sections, a total of 14 unique inorganic minerals were identified in Raman spectra including quartz, dolomite, calcite, hematite and anhydrite. Shale thin sections tended to be dominated by organic material. OM was often observed mixed with inorganic minerals. Sand- and mudstones were dominated by inorganic minerals. The PLS extrapolated the post-mature set to reflectances >1.2%. The study set ranged from very immature to postmature in the median of map fit-peak parameters. However, point maturity maps indicate that matrix OM in all study samples is immature and that discreet organic particles selected for mapping, which may be inertinites, bias medians towards more-mature. The work demonstrates the capabilities of RMS to perform both whole-slide mineralogy and OM analysis with applications to formation evaluation in oil & gas, carbon sequestration and mining. Here, analysis of sealing formations in the well indicates high levels of immature organic matter that would not be a viable target for future oil production that could compromise the CO2 storage site. The work brings together diverse disciplines from geology and petrography to analytical chemistry, big data and microscopy.
Oil Sands and Mature Fine Tailings: Oil sand reserves are a major source of oil for the United States. Oil sands are a mixture of sand, clay, water, and bitumen. The refining process requires large volumes of water and generates hazardous Mature Fine Tailings (MFTs) that are stored in engineered settling ponds. They are of major environmental concern due to their persistence and difficulty to naturally biodegrade. MFT Contaminants of Concern: Naphthenic Acids (NAs), Polycyclic Aromatic Hydrocarbons (PAHs), Benzene, Toluene, Ethylbenzene and Xylene (BTEX), Metals, Residual Bitumen. BioTiger{sup TM} (BT{sup TM}), the SRNL patented 12 component microbial consortia was found to cometabolically degrade some NAs and PAHs. Previous studies performing short term exposure (48 hours and 7 days) to BT{sup TM} have resulted in increased toxicity due to the partial degradation of PAHs forming toxic intermediates. Objective: Evaluate the ecotoxicity of BT{sup TM} remediated MFTs exposed to a 2 week period w/ yeast (Y) extract. This work will determine BT{sup TM}'s remediation of MFTs from Fort McMurray, Alberta. Acute toxicity tests will be performed under section 9 of EPA's Method for Measuring Acute Toxicity using the freshwater organism, Ceriodaphnia dubia. Monitor BT{sup TM} growth through Most Probable Number (MPN) counts, pH, and metal bioavailability will also be evaluated. Preparing tailing solutions for biodegradation: BT{sup TM} components were grown in R2A media and combined. Mother BT{sup TM} was centrifuged at 7000 rpm for 20 minutes and resuspended in Bushnell Haus. 33 g of tailings were added to 1100 mL Bushnell Haus along with yeast extract (11 g) to create a 3% tailing solution. Treatments were performed in triplicate. Preparing solutions for toxicity tests using C. dubia: Supernatant was collected immediately after centrifuging at 7000 rpm for 20 min. Supernatant was filtered via a 0.22 μm sterile system. All treatments except MFT, Y peaked at T=4. This decrease in microbial growth could be associated with toxicity from intermediate byproducts. Treatments containing only MFTs decreased in the initial 11 days before growing significantly. Final solution for MFT, Y treatment had the highest pH. This could potentially be due to increased microbial activity linked with yeast consumption. All treatments except MFT, Y peaked at T=4. This decrease in microbial growth could be associated with toxicity from intermediate byproducts. Treatments containing only MFTs decreased in the initial 11 days before growing significantly. Future Direction: Await results from Acute Toxicity Tests and Metal Bioavailability Quantification of biosurfactant production. Evaluate hydrocarbon degradation byproducts using an analytical chemistry approach. More toxicity experiments with variations in time and conditions.
In December of 2023 a shipment of commercially irradiated fuel rods from the Byron Generating Station in Illinois was successfully shipped to the Materials and Fuels Complex (MFC) at Idaho National Laboratory (INL). The make-up of the rods includes a mix of cladding types from traditional ZirloTM, advanced zirconium alloys, and chrome coated ZirloTM. Burnups range from regular end of life values to over 70 GWd/MTU rod average. The R&D plan for the rods involves multiple projects from developing licensing data for new claddings to integral transient tests to support burnup extension efforts in the United States. The R&D began in early 2024 with the nondestructive examinations of the rods after which they will be sectioned for microscopy, mechanical testing, and analytical chemistry. Additionally, many rod segments will be refabricated into new test pins and inserted into a static water capsule for integral Reactivity Initiated Accident (RIA) and Loss of Coolant Accident (LOCA) testing at the TREAT reactor.
Throughout the centuries, as man has become increasingly affluent, his interest in antiquities and objects of art, and the price he has been willing to pay for them, has increased. Inevitably, one result has been to attract the unscrupulous to the production and sale of counterfeit paintings, sculptures, and other works of art. The skill of forgers varies but often is highly sophisticated. However, dealers, museum curators, and other experts have also become more skillful in the detection of forgeries. Scientific tools of increasing sensitivity and sophistication have gradually been applied to the examination of the materials of art and archaeology. Such tools frequently support and render more reliable the judgment of the experts. The quality of forgeries may improve further as their makers become acquainted with the new methods of detection and in turn learn to circumvent or confound the methods. Therefore, the development of still more advanced methods of examination has great utility in the art world. This is particularly true if the ultimate effect is to make circumvention of the methods of examination so costly that the economic incentives for producing forgeries may be substantially reduced, if not eliminated.
Impurities present in commercially available halide perovskite precursors are known to affect photovoltaic performance. Here, we employ bulk single crystal growth of FAPbI 3 using solvent orthogonality induced crystallization (SONIC) to remove a broad set of extrinsic impurities from commercially available halide perovskite precursors, as verified by detailed chemical analysis. Following SONIC purification, FAPbI 3 films made from PbI 2 of originally low purity (99%) and high purity (99.99%) show improved phase purity and stability under light and heat relative to films made from raw precursors or precursors purified via retrograde powder crystallization (RPC) in 2-methoxyethanol, a method commonly utilized in recent reports of the highest-efficiency perovskite solar cells. In conclusion, single-crystal purification of precursors improves film stability under operational stressors, and the large enhancements in material purity provide a cleaner slate for improved isolation of compositional and additive effects on perovskite phase stability.
Studying the effect of resin RI on print fidelity. Chemically modifying RI resins to demonstrate 3D structures print without height limitation resulting on ceramic and nonceramic print as tall as 2.5 mm with sub-micron features.
To date, chemical security education practices in postsecondary institutions are poorly understood. The purpose of this study is to provide an initial understanding of the practices, attitudes, and barriers toward chemical security education for undergraduate and graduate programs in the United States (US) by surveying representatives of American Chemical Society (ACS)-approved programs. All programs with ACS-approved undergraduate chemistry programs (n = 691) were contacted for participation: 21% (n = 148) fully completed and 6% (n = 41) partially completed the survey for a combined total of 27% complete and/or partially complete surveys (n = 189). We observed that most programs currently teach chemical safety (undergraduate >99%, graduate 73%); however, only about one-third of programs teach chemical security at any education level (undergraduate 32%, graduate 34%). We also observed that safety education is provided more frequently than security education. Further, ACS-approved programs reported that their chemical safety culture was stronger than chemical security culture and felt that safety should be taught differently than security. The overwhelming majority of respondents (96%) indicated that chemical safety should be mandatory at some level, while only about half of respondents (57%) indicated that chemical security should be mandatory at some level. More efforts are needed by the chemistry community to raise awareness of the importance of chemical security education so that more institutions commit to training their faculty and students on the topic. The authors suggest that adoption of chemical security education could be increased if ACS were to advocate for chemical security by including it in its guidelines for educational program approval.
Here in this special collection dedicated to Prof. Jean-Michel Savéant, we report on the synthesis and characterization of a novel binuclear Fe(III) fused porphyrin. Ultraviolet-visible spectroscopy confirms the extended electronic structure of this macrocycle. In addition, Fourier transform infrared spectroscopy indicates the Fe centers experience a relatively rigid ligand environment as compared to a structurally related mononuclear complex featuring an 18 π-aromatic porphyrin ligand. X-ray photoelectron and X-ray absorption near edge spectroscopies confirm the iron centers of both assemblies are Fe(III) in the as prepared, resting state. In comparison with the mononuclear porphyrin, electrochemical measurements show there is a doubling of the number of redox events associated with the fused, binuclear complex. In conclusion, key features of the fused-iron-porphyrin include: 1) bimetallic-iron sites, 2) a π-extended ligand capable of delocalizing electrons across the multimetallic scaffold, and 3) the ability to store up to six electrons.
Abstract The one-step breakdown and derivatization of a panel of nine fentanyls to yield uniquely tagged products that can be detected by Electron Ionization Gas Chromatography-Mass Spectrometry (EI-GC-MS) is presented. The method involves the treatment of the synthetic opioids with 2,2,2-trichloroethoxycarbonyl chloride (TrocCl) at 60 °C for 3 h in dichloromethane and furnishes two products from one fentanyl molecule that can be used to retrospectively identify the original opioid. Parameters that were studied and fully optimized for the method included temperature, solvent, nature of scavenging base and reaction time. One of the two resulting products from the reaction bears the trichloroethoxycarbonyl (Troc) tag attached to the norfentanyl portion of the original opioid and greatly aids in the opioid detection and identification process. The methodology has been applied to the chemical modification of a panel of nine fentanyls and in all cases the molecular ion peak for the Troc-norfentanyl product bearing the distinctive trichloroethyl isotopic signature can be clearly observed. The method’s LLOD was determined to be 10 ng/mL while its LLOQ was found to be 20 ng/mL. This methodology represents the first application of chloroformates in the chemical modification of this class of synthetic opioids that are notoriously inert to common derivatization strategies available for GC–MS analysis.