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At least 343 records · Page 19

Review of ECCS Acceptance Criteria and Experimental Basis Evolution Toward Fuel Fragmentation, Relocation, and Dispersal Studies

The U.S. nuclear industry is pursuing extensions of light water reactor (LWR) fuel burnup and enrichment limits to approximately 75 GWd/t and 10 wt.% 235 U to achieve economic and operational benefits. A central safety consideration in this effort is the behavior of high burnup (HBu) fuel during loss-of-coolant accidents (LOCAs), particularly fuel fragmentation, relocation, and dispersal (FFRD). Here, this work provides a historical and technical review of U.S. LOCA regulation and experimentation, clarifying how the evolution of Emergency Core Cooling System (ECCS) acceptance criteria in 10 CFR 50.46 has shaped both testing approaches and interpretations of fuel safety. The study revisits the original intent of the ECCS criteria, showing that the peak cladding temperature and equivalent cladding reacted limits were developed as surrogates to preserve a coolable geometry. The explicit inclusion of the coolable geometry criterion in the regulation was intended to emphasize the underlying safety philosophy and as a safeguard against unforeseen failure modes, an intent that remains directly relevant to modern concerns regarding FFRD. The review traces the lineage of HBu LOCA experiments to the Argonne National Laboratory furnace tests, from which subsequent programs at Studsvik, Halden, and Oak Ridge National Laboratory were derived. These tests employed a 5 °C/s heating rate inherited from early embrittlement studies, a stylized temperature history that does not represent actual LWR LOCA thermal-hydraulics. Comparison of these test conditions to pressurized water reactor large break LOCAs and separate effects data indicates that the existing HBu LOCA database may not be fully applicable to all LWR LOCA scenarios, from which a qualitative framework for applicability is proposed.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Simulated Performance of the Micro-Pocket Fission Detector in the Advanced Test Reactor Critical Facility

The Micro-Pocket Fission Detector (MPFD) is a small-form–factor real-time fission chamber. MPFD performance has been simulated in the Advanced Test Reactor Critical Facility (ATRC), located at Idaho National Laboratory (INL). Here, the neutron and gamma-ray flux profiles and magnitudes were simulated using Monte Carlo N-Particle (MCNP) in the near-core B-8 irradiation position. These simulations were performed at 69 discrete axial locations inside the B-8 position for three separate orientations of the nearby hafnium outer shim control cylinders and at a power level of 700 Wth. The resulting neutron and gamma-ray flux values were used to determine the MPFD response for various fissile masses and detector gas pressures. The optimal gas-operating pressure was determined to be between 30 and 60 psig. The required fissile-layer mass was determined to be between 1–2 µg of 235 U. Additionally, the gamma-ray to fission-fragment interaction rate was determined to be 4.42 × 10 -3 with average energy deposition for gamma rays and fission fragments in 30 psig argon gas to be 1 keV and 9.5 MeV, respectively.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Brush seal bristle flexure and hard-rub characteristics

The bristles of a 38.1-mm (1.5-in) diameter brush seal were flexed by a tapered, 40-tooth rotor operating at 2600 rpm that provided sharp leading-edge impact of the bristles with hard rubbing of the rotor lands. Three separate tests were run with the same brush accumulating over 1.3 x 10(exp 9) flexure cycles while deteriorating 0.2 mm (0.008 in) radially. In each, the test bristle incursion depth varied from 0.130 to 0.025 mm (0.005 to 0.001 in) or less (start to stop), and in the third test the rotor was set 0.25 mm (0.010 in) eccentric. Runout varied from 0.025 to 0.076 mm (0.001 to 0.003 in) radially. The bristles wore but did not pull out, fracture, or fragment. Bristle and rotor wear debris were deposited as very fine, nearly amorphous, highly porous materials at the rotor groove leading edges and within the rotor grooves. The land leading edges showed irregular wear and the beginning of a convergent groove that exhibited sharp, detailed wear at the land trailing edges. Surface grooving, burnishing, 'whipping,' and hot spots and streaks were found. With a smooth-plug rotor post-test leakage increased 30 percent over pretest leakage.

Hendricks, Robert C.↗

Brush seal low surface speed hard-rub characteristics

The bristles of a 38.1-mm (1.5-in.) diameter brush seal were flexed by a tapered, 40-tooth rotor operating at 2600 rpm that provided sharp leading-edge impact of the bristles with hard rubbing of the rotor lands. Three separate tests were run with the same brush accumulating over 1.3 x 10(exp 9) flexure cycles while deteriorating 0.2 mm (0.008 in.) radially. In each, the test bristle incursion depth varied from 0.130 to 0.025 mm (0.005 to 0.001 in.) or less (start to stop), and in the third test the rotor was set 0.25 mm (0.010 in.) eccentric. Runout varied from 0.025 to 0.076 mm (0.001 to 0.003 in.) radially. The bristles wore but did not pull out, fracture, or fragment. Bristle and rotor wear debris were deposited as very fine, nearly amorphous, highly porous materials at the rotor groove leading edges and within the rotor grooves. The land leading edges showed irregular wear and the beginning of a convergent groove that exhibited sharp, detailed wear at the land trailing edges. Surface grooving, burnishing, 'whipping,' and hot spots and streaks were found. With a smooth-plug rotor, post-test leakage increased 30 percent over pretest leakage.

Hendricks, Robert C.↗

Brush seal low surface speed hard-rub characteristics

The bristles of a 38.1-mm (1.5-in.) diameter brush seal were flexed by a tapered, 40-tooth rotor operating at 2600 rpm that provided sharp leading-edge impact of the bristles with hard rubbing of the rotor lands. Three separate tests were run with the same brush accumulating over 1.3 x 10(exp 9) flexure cycles while deteriorating 0.2 mm (0.008 in.) radially. In each, the test bristle incursion depth varied from 0.130 to 0.025 mm (0.005 to 0.001 in.) or less (start to stop), and in the third test the rotor was set 0.25 mm (0.010 in.) eccentric. Runout varied from 0.025 to 0.076 mm (0.001 to 0.003 in.) radially. The bristles wore but did not pull out, fracture, or fragment. Bristle and rotor wear debris were deposited as very fine, nearly amorphous, highly porous materials at the rotor groove leading edges and within the rotor grooves. The land leading edges showed irregular wear and the beginning of a convergent groove that exhibited sharp, detailed wear at the land trailing edges. Surface grooving, burnishing, 'whipping,' and hot spots and streaks were found. With a smooth-plug rotor, post-test leakage increased 30 percent over pretest leakage.

Hendricks, Robert C.↗

Brush seal bristle flexure and hard-rub characteristics

The bristles of a 38.1-mm (1.5-in.) diameter brush seal were flexed by a tapered, 40-tooth rotor operating at 2600 rpm that provided sharp leading-edge impact of the bristles with hard rubbing of the rotor lands. Three separate tests were run with the same brush accumulating over 1.3 x 10(exp 9) flexure cycles while deteriorating 0.2 mm (0.008 in.) radially. In each, the test bristle incursion depth varied from 0.130 to 0.025 mm (0.005 to 0.001 in.) or less (start to stop), and in the third test the rotor was set 0.25 mm (0.010 in.) eccentric. Runout varied from 0.025 to 0.076 mm (0.001 to 0.003 in.) radially. The bristles wore but did not pull out, fracture, or fragment. Bristle and rotor wear debris were deposited as very fine, nearly amorphous, highly porous materials at the rotor groove leading edges and within the rotor grooves. The land leading edges showed irregular wear and the beginning of a convergent groove that exhibited sharp, detailed wear at the land trailing edges. Surface grooving, burnishing, 'whipping', and hot spots and streaks were found. With a smooth-plug rotor, post-test leakage increased 30 percent over pretest leakage.

Hendricks, Robert C.↗

On the collapse and violent relaxation of protoglobular clusters

During the formation of stellar systems such as globular clusters, low-mass subcondensations which eventually form stars must retain a geometric size throughout the collapse process that is small compared to the characteristic distance separating them. If the local velocity dispersion of the subcondensations is small, the overall dimension of the system can decrease substantially before reaching a dynamical equilibrium state. The maximum collapse factor is deduced by examining the growth of the velocity dispersion and the spread in arrival times at the origin caused by local and global fluctuations. It is shown, analytically as well as in a series of N-body simulations, that the maximum reduction in the characteristic dimension of a system of N fragments with an initial homogeneous distribution subject to N exp 1/2 fluctuations is proportional to N exp 1/3. Direct physical collisions between low-mass subcondensations are therefore unlikely to occur in protoglobular clusters. The results are discussed in the context of fragmentation and violent relaxation.

Aarseth, S. J.↗

Measurement of isolated-photon plus two-jet production in p p collisions at s = 13 TeV with the ATLAS detector

The dynamics of isolated-photon plus two-jet production in pp collisions at a centre-of-mass energy of 13 TeV are studied with the ATLAS detector at the LHC using a dataset corresponding to an integrated luminosity of 36.1 fb−1. Cross sections are measured as functions of a variety of observables, including angular correlations and invariant masses of the objects in the final state, γ+jet+jet. Measurements are also performed in phase-space regions enriched in each of the two underlying physical mechanisms, namely direct and fragmentation processes. The measurements cover the range of photon (jet) transverse momenta from 150 GeV (100 GeV) to 2 TeV. The tree-level plus parton-shower predictions from SHERPA and PYTHIA as well as the next-to-leading-order QCD predictions from SHERPA are compared with the measurements. The next-to-leading-order QCD predictions describe the data adequately in shape and normalisation except for regions of phase space such as those with high values of the invariant mass or rapidity separation of the two jets, where the predictions overestimate the data.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Inorganic analyses of Martian surface samples at the Viking landing sites

Elemental analyses of fines in the Martian regolith at two widely separated landing sites, Chryse Planitia and Utopia Planitia, produced remarkably similar results. At both sites, the uppermost regolith contains abundant Si and Fe, with significant concentrations of Mg, Al, S, Ca, and Ti. The S concentration is one to two orders of magnitude higher, and K (less than 0.25% by weight) is at least 5 times lower than the average for earth's crust. The trace elements Sr, Y, and possibly Zr have been detected at concentrations near or below 100 parts per million. Pebble-sized fragments sampled at Chryse contain more S than the bulk fines and are thought to be pieces of a sulfate-cemented duricrust.

Clark, B. C.↗

X-Ray Computed Tomography During Preliminary Examination of Apollo Drive Tube 73001

Introduction: Starting in 2019, the Apollo Next Generation Sample Analysis (ANGSA) Program has enabled consortium studies of specially curated Apollo samples that were previously unstudied (or under studied). This began with unsealed core tube 73002 [1,2] that is the upper part of a station 3 double drive tube. More recently the pro-gram extended to the study of a variety of frozen Apollo 17 samples [3], as well as the gas extraction [4] and dis-section [5] of 73001, the lower half of the station 3 double drive tube, that was sealed under vacuum on the Moon. In this abstract we will examine the role of X-ray Computed Tomography (XCT) during the preliminary examination process for sealed core 73001, including: (1) engineering scans to aid in understanding the gas extraction process, whole-core scanning prior to opening to inform extrusion and dissection work, and (3) individual particle scanning to characterize rock fragment lithologies for follow on studies. Methodology: Sample 73001 is a 33 cm long, 4 cm diameter regolith sample collected inside a drive tube (~1 mm aluminum walls). That drive tube was sealed inside a 0.5 mm thick stainless steel (SS) Core Sample Vacuum Container (CSVC). XCT scans for engineering purposes were done on the Nikon XTH 320 system at Johnson Space Center using the 225 kV multi-metal reflection source at 215 kV, 179 A, and a 38.49 m voxel size. Individual >4 mm particles separated from the core during processing (then triply sealed in Teflon bags) were also scanned at JSC using the 180 kV source at 90 kV, 33 A, and a 2.98 – 10.65 m voxel size. Whole-core scans were done at the University of Texas High-Resolution X-ray Computed Tomography Facility (UTCT) on the 225 kV reflection source on the North Star Imaging cabinet XCT system. These scans included: (1) a series of 9 overlapping super-resolution scans each covering a ~4 cm length of the tube at 190 kV, 180 µA, and a 12.9 µm voxel size and (2) a lower resolution continuous helical scan of the entire core at 190 kV, 180 µA, and a 51.8 µm voxel size. Progress and Results: Before piercing and extracting the gas from sample 73001, an XCT scan of the bottom portion of the CSVC was used to confirm the location of the Teflon cap on the inner drive tube, to ensure it was not accidentally pierced during gas extraction. Similarly, after piercing, the bottom and top portions of the CSVC were scanned in order to capture engineering knowledge about the results of the piercing process, as well as the metal knife edge vacuum seal (SS into In-Ag alloy). Both scans will provide constraints on future work of this type, particularly for samples collected during the Artemis mission. Another finding from these "engineering" scans was that the device in the drive tube that immobilizes the regolith (the keeper) was not seated in the tube properly. This meant that (1) the drive tube could not be removed from the CSVC for the trip to UTCT, and (2) the procedure for opening and extruding the drive tube had to be modified. Had either of these things not been known prior to opening the CSVC, it could have led to an inability to XCT scan the whole core at high resolution and/or potential disruption of the core stratigraphy during extrusion. At UTCT, the entire length of the core was scanned at high resolution (12.9 microns per voxel). This scan serves multiple purposes: (1) A lower resolution (and uncorrected) version of these scans stitched together was used to help inform the processors of potential pitfalls during extrusion and dissection; and (2) the full resolution corrected data will serve as the permanent in situ record of the stratigraphy of the sample and will enable future researchers to perform a variety of analyses. So far, 92 of the 121 >4 mm particles separated during dissection pass 1 of sample 73001 have been individually scanned. These scans clearly show the lithology of each particle while keeping the particles in pristine condition. Because of the dust adhering to particle exteriors it would otherwise be impossible to determine lithologies in a non-contaminating way. Thus far the types of lithologies seen in sample 73001 (e.g., regolith breccias, impact-melt breccias, agglutinates, and basalts) are similar to those previously identified in sample 73002 [2]. By the time of the meeting, all particles from all 3 dissection passes will have been scanned and statistics on the different lithologies in 73001 compiled. References: [1] Shearer et al. (2020) 51st LPSC, abstract 1181. [2] Zeigler et al. (2020) 51st LPSC, abstract 3023. [3] Kent et al. (2022) This Volume. [4] McDonald et al. (2022) European Lunar Symposium. [5] Gross et al (2022) This volume.

Moon↗

Fragments of quartz monzodiorite and felsite in Apollo 14 soil particles

Samples of 'evolved' lithologies, felsite, quartz monzodiorite (QMD), and whitlockite-rich quartz monzodiorite, were identified compositionally and petrographically among 2-4-mm soil particles from Apollo 14. Fragments of QMD were found to be extremely rare in the Apollo 14 samples. Felsite is similar to previously reported samples. QMD 14161,7069 is similar to 15405 QMD and has ITE concentrations in KREEP-like concentration ratios of about twice the ITE concentrations of average high-K KREEP. QMD cumulate has the highest measured REE concentrations of any lunar sample to date with the exception of individual whitlockite grains. Felsite and whitlockite-rich lithologies appear to be petrogenetically related and have complementary compositions representing separated fractions of the QMD or KREEP-like parental melt. Felsite is a silica-rich fraction of the residual liquid or it is a derivative of the silica-rich fraction. Felsite or lunar granite of this type results from residual liquid separation following crystal-liquid separation of a QMD-like parent melt with concentration ratios of ITEs similar to those of KREEP.

Jolliff, B. L.↗

2025 ASMS Investigation of the Collision-Induced Dissociation Mechanism of Protonated TODGA with IRIS

Title (20 words): Investigation of the Collision-Induced Dissociation Mechanism of Protonated TODGA with IRIS Introduction (120 words): One of the challenges facing wide-spread adoption of nuclear power is the development of efficient separation processes for used nuclear fuel. The molecules in separation processes are subjected to an extreme environment due to the high radiation fields from the used fuel and highly acidic media used for fuel dissolution, which results in significant molecular degradation, leading to reduced process efficiency. These degradation products must be identified and studied so mitigation strategies can be developed to maintain process efficiency. However, complex systems can have many degradation products, complicating identification. Untargeted analysis tools could be used to understand radiation chemistry in complex systems. However, this would necessitate improved understanding of the gas-phase fragmentation mechanisms of fuel cycle molecules like tetraoctyldiglycolamide (TODGA). Methods (120 words): The gas-phase fragmentation of protonated TODGA was investigated using collision-induced dissociation (CID), resonance ejection, and infrared ion spectroscopy (IRIS). CID and resonance ejection experiments were conducted using a Bruker Daltonics (Bremen, Gemany) SolariX XR fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer. IRIS spectra of protonated TODGA and its two CID fragmentation products were measured using a modified Bruker amaZon Speed ETD 3D quadrupole ion trap mass spectrometer coupled to the Free Electron Lasers for Infrared eXperiments (FELIX) free electron laser. Measured spectra were compared with density functional theory (DFT) calculations using the Gaussian 16, Revision C.02 software package with the ?B97X-D functional and def2-TZVPP basis sets. Candidate structures were generated using the CREST 3.0 conformational sampling software tool. Preliminary Data (300 words): Collision-induced dissociation of protonated TODGA ([C36H73N2O3]+, m/z=581.562) results two fragment ions, one at m/z=340.285 assigned as [C20H38NO3]+ and the other at m/z=312.290, assigned as [C19H38NO2]+. Based on the assigned formula and the structure of protonated TODGA, the fragment at m/z=340.285 is likely formed from elimination of neutral dioctylamine. Comparison of the IRIS spectrum of m/z=340.285 with DFT predictions suggests it contains a ring structure, and is assigned as N-octyl-N-(6-oxo-1,4-dioxan-2-ylidene)octan-1-aminium. Based on this structure and the structure of protonated TODGA, we hypothesize this fragment formed from elimination of neutral dioctylamine followed by a ring closure mechanism. Comparison of the IRIS spectrum of the fragment at m/z=312.290 with DFT predictions also indicated the presence of a ring structure, assigned as N-(1,3-dioxolan-4-ylidene)-N-octyloctan-1-aminium. This product could be formed from elimination of carbon monoxide from the ring of m/z=340.285 as a sequential fragmentation or formed directly from protonated TODGA via elimination of neutral N,N-dioctylformamide followed by a ring closure. Resonance ejection experiments where m/z=340 was continuously ejected from the IRC cell showed no decrease in intensity of m/z=312.290 across several collision energies, suggesting that the later, direct formation mechanism, dominates. The location of the ionizing proton in protonated TODGA is important for modeling the fragmentation mechanisms. DFT calculations suggested that the position of bands involving the coupled vibrations of the amide C—N and C=O bonds in TODGA are the most sensitive to proton location. Evaluation of the IRIS spectrum of protonated TODGA suggests that the ionizing proton is located between the two amid oxygens. This protonation location was calculated to lie approximately 30 kJ/mol lower in energy than the next lowest energy location, with the proton located solely on one of the amide oxygens. Novel aspect (20 words): Infrared ion spectroscopy combined with resonance ejection experiments and density functional theory to probe the collision-induced dissociation mechanism of tetraoctyldiglycolamide.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗

GRM crustal magnetic anomalies: Separating the Lord Howe Rise and Norfolk Ridge submarine structures

Multiple source bodies often lie within the resolution element of the MAGSAT and POGO data. Small weak sources lying near larger stronger sources will tend to be missed, although they do contribute to the total observed anomaly. Lower elevation magnetic anomaly surveys such as GRM alleviate this problem through the combined effects of significantly greater resolution and stronger signal amplitude. This permits the detection of smaller source bodies, and analysis of their structure and nature. The improvement a GRM will provide is demonstrated in the Lord Howe Rise/Norfolk Ridge area east of Australia, between the Tasman Sea and south Fiji Basin. The submarine features origin have important plate tectonic implications. The Lord Howe Rise (LHR) is a continental fragment broken off from Australia by the opening of the Tasman Sea. It is a wide, shallow structure lying between 160 and 165 deg longitude at 23 to 37 deg S latitude. Seismic refraction data show the LHR crust extending to depths in excess of 20 km.

Frey, H.↗

High-dimensional isotomics, part 2: Observations of over 100 constraints on methionine's isotome

The abundances of different isotopic forms of a compound, or isotopologues, will vary based on its physical and chemical history. The number of isotopologues increases combinatorically with the size of a molecule, and even small molecules such as amino acids have thousands of potentially observable isotopic variants. However, due to the analytical challenges of separating and observing isotopologues, only a few dimensions of isotopic diversity are routinely measured. Overcoming these challenges requires both an experimental method to observe many isotopic properties and a theoretical framework for interpreting these experiments. In Part 1, we presented such a theoretical framework; here, we demonstrate an experimental method, which we apply to methionine. Our approach uses a Q Exactive HF Orbitrap to perform several “M + N experiments”, where a sample is ionized, a subset of its isotopologues with cardinal mass N daltons greater than the unsubstituted isotopologue is selected and fragmented, and the proportions of all detectable isotopic forms of those fragment ions are quantified. We perform M + 1, M + 2, M + 3, and M + 4 experiments of a methionine sample and standard where the sample has a 100 ‰ enrichment of 13C at the methyl carbon relative to the natural 13C abundance at that position in the standard, and is otherwise identical to the standard. We observe isotopic forms of 8 fragment ion species for each version of the M + N experiment. With the assistance of a forward model of expected mass spectra, we identify isotopic peaks for each fragment ion based on observed mass and abundance, screen these for data quality, and quantify abundances for 146 unique isotopic peaks at precisions of ≈ 0.3–3 ‰. We present our direct observations and use them to reconstruct the concentrations of 19 individual singly, doubly, and triply-substituted isotopologues; doing so gives fewer constraints and broader error bars than working with the direct observations, but may be more interpretable for some applications. We also examine possibilities for measuring additional peaks, which are primarily limited by the detection limit of the Orbitrap-IRMS method. We then suggest some possible uses of our direct measurements for chemical forensics and hypothesis testing. Furthermore, our results demonstrate the diversity of isotopic constraints currently observable and interpretable for organic molecules.

58 GEOSCIENCES↗

Stable and Recyclable Photocatalysts of CsPbBr 3 @MSNs Nanocomposites for Photoinduced Electron Transfer RAFT Polymerization

All-inorganic metal halide perovskite CsPbX 3 (X = Cl, Br, I) nanocrystals (NCs) have demonstrated attractive optoelectronic characteristics. However, their photocatalytic properties are limited by their poor stability and easy recombination of photogenerated carriers. Herein, we introduced a CsPbBr 3 @MSNs nanocomposite (CsPbBr 3 NCs embedded in dendritic mesoporous silica nanospheres (MSNs)) as photocatalysts for photoinduced electron transfer reversible addition–fragmentation chain transfer (PET-RAFT) polymerization. In this study, the CsPbBr 3 nanocrystals (~8.1 nm; PLQY of 62 ± 2.1%) were embedded in dendritic MSNs using a nanoconfinement strategy. PET-RAFT polymerization was successfully initiated using the CsPbBr 3 @MSNs nanocomposite as the photocatalyst. Reaction variables, such as catalyst loading, monomer composition, and excitation light wavelengths, were varied to yield polymers with the desired control of molecular weight and dispersity as well as block copolymers with high chain-end fidelity. In addition, the perovskite-based photocatalysts could be readily separated and purified, which allowed effective and rapid recycling of the nanocomposites for multiple polymerization cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

2MASS J15491331-3539118: a new low-mass wide companionof the GQ Lup system

Substellar companions at wide separation around stars hosting planets or brown dwarfs (BDs) yet close enough for their formation in the circumstellar disc are of special interest. In this Letter we report the discovery of a wide (projected separation ~16".0, or 2400AU, and position angle 114.61°) companion of the GQLup A-B system, most likely gravitationally bound to it. A VLT/X-shooter spectrum shows that this star, 2MASS J15491331-3539118, is a bonafide low-mass (~0.15 M(ʘ) ) young stellar object (YSO) with stellar and accretion/ejection properties typical of Lupus YSOs of similar mass, and with kinematics consistent with that of the GQLup A-B system. A possible scenario for the formation of the triple system is that GQ Lup A and 2MASS J15491331-3539118 formed by fragmentation of a turbulent core in the Lup I filament, while GQ Lup B, the BD companion of GQ Lup A at 0".7, formed in situ by the fragmentation of the circumprimary disc. The recent discoveries that stars form along cloud filaments would favour the scenario of turbulent fragmentation for the formation of GQ Lup A and 2MASS J15491331-3539118.

J. M. Alcalá↗

Design and Evaluation of a Gas Chromatograph-Atmospheric Pressure Chemical Ionization Interface for an Exactive Orbitrap Mass Spectrometer

Various separation and mass spectrometric (MS) techniques have furthered our ability to study complex mixtures, and the desire to measure every analyte in a system is of continual interest. For many complex mixtures, such as the total molecular content of a cell, it is becoming apparent that no one single separation technique or analysis is likely to achieve this goal. Therefore, having a variety of tools to measure the complexity of these mixtures is prudent. Orbitrap MSs are broadly used in systems biology studies due to their unique performance characteristics. However, GC-Orbitraps have only recently become available, and instruments that can use gas chromatography (GC) cannot use liquid chromatography (LC) and vice versa. This limits small molecule analyses, such as those that would be employed for metabolomics, lipidomics, or toxicological studies. Thus, a simple, temporary interface was designed for a GC and Thermo Scientific™ Ion Max housing unit. This interface enables either GC or LC separation to be used on the same MS, an Exactive™ Plus Orbitrap, and utilizes an atmospheric pressure chemical ionization (APCI) source. The GC-APCI interface was tested against a commercially available atmospheric pressure photoionization (APPI) interface for three types of analytes that span the breadth of typical GC analyses: fatty acid methyl esters (FAMEs), polyaromatic hydrocarbons (PAHs), and saturated hydrocarbons. The GC-APCI-Orbitrap had similar or improved performance to the APPI and other reported methods in that it had a lower limit of quantitation, better signal to noise, and lower tendency to fragment analytes. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗