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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Investigation of Effects of SiO{sub 2} Content and Cooling Rate on Crystallization in Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} System Using In Situ Confocal Laser Scanning Microscopy

The crystallization behaviors of the Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} system in a non-equilibrium state with various chemical compositions and cooling rates were investigated by confocal laser scanning. Equilibrium samples were prepared in melt states and cooled at a rate of 1 K/min to produce samples in quasi-equilibrium states. The effect of SiO{sub 2} on the phase constitution was investigated using Image Analyzer, and the changes of the phase ratios were analyzed using activity values of Fe{sub 2}O{sub 3} calculated using FactSage 7.1. The Continuous cooling transformation diagram of the Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} system was obtained for various cooling rates. The temperatures at which the primary phase formed for various SiO{sub 2} contents and cooling rates differed from the equilibrium temperatures, and the phase-formation temperature ranges varied with the cooling rate. In addition, the reduction degree of each sample was measured to determine the effect of SiO{sub 2} content and cooling rate on the Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} system. The reduction degree in the FeO{sub 3}-CaO-SiO{sub 2} system is dominantly influenced by the SiO{sub 2} bond-phase morphology (CF, C{sub 2}S, C{sub 3}S, or glass) rather than the cooling rate.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Low Solution Temperature Heat Treatment of AlSi{sub 9}Cu{sub 3}(Fe) High-Pressure Die-Casting Actual Automotive Components

Usually, high-pressure die-casting (HPDC) components cannot be heat-treated at high temperature without the occurrence of surface blisters, which are unacceptable for surface finish and may reduce the mechanical properties. In this context, the purpose of the present paper was to analyze the effectiveness of special low solution temperature T6 heat treatment in overcoming this limit for HPDC AlSi{sub 9}Cu{sub 3} alloy. Very low solution temperatures (< 450 °C, followed by 165 °C aging) to prevent the occurrence of blisters were combined with commonly used times (from 1 to 16 h) ensuring the feasibility of industrial application. Treatments were conducted on samples extracted from actual castings to evaluate the typical defects encountered in common production. Properties were analyzed by means of visual inspection, microstructural observations, image analysis, hardness, tensile tests and fractography. The results showed that it is possible to use solubilization temperatures below 450 °C for several hours in a T6 treatment to give strengthening without relevant blistering in AlSi{sub 9}Cu{sub 3} alloy. The optimum match of properties was provided by a solution treatment at 430 °C for 4 h followed by an aging at 165 °C for 8 h, which gave a yield increase of ~ 50 MPa, an increase in ductility and the best Quality Index value.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Experimental Assessment of High Heating Rates in Induction Heating with Temperature-Sensitive Lacquers

The fast evolving temperature fields at the surface of induction-heated parts were measured by a contactless, optical method based on temperature-sensitive lacquers recorded with a high-speed imaging system. The positions of specific isotherms over time were precisely measured by image analysis. A 4340 steel cylinder and two spur gears of the same material were investigated. One spur gear was treated at high frequency, and the other one at simultaneous dual frequency. In both cases, the temperature started to rise at the root of the teeth and then expanded along the flanks. The heating rates were higher at the tips than at the roots for both treatments, with higher values for the dual-frequency treatment. The layer of transformed material was similar for both treatments, but the transformation temperature varied greatly. It was found to be 50-100 °C higher than the equilibrium values, depending on the local heating rate.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effects of Vanadium on Modification of Iron-Rich Intermetallics and Mechanical Properties in A356 Cast Alloys with 1.5 wt.% Fe

Formation of Fe-rich intermetallics and mechanical properties of vanadium-modified A356 cast alloys with 1.5 wt.% Fe were investigated using image analysis, scanning electron microscopy, differential scanning calorimetry, and a tensile test. The results showed that V content has no apparent influence on α-Al grain size in A356 alloys with high Fe content. Also, 0.8 wt.% V is beneficial for improving mechanical properties in A356 cast alloys with high Fe content. Specifically, these results can be attributed to the formation of Chinese script or block α-Fe phases, refined needle-like β-Fe (Al{sub 5}FeSi), and decreased porosities. An excessive amount of V deteriorates mechanical properties of alloys because it leads to VSi{sub 2} formation, large sized iron-rich intermetallics, and increased porosities.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Quality Assessment of Al Castings Produced in Sand Molds Using Image and CT Analyses

Nowadays, the economic production of aluminum casts is becoming increasingly important. Therefore, the decision of whether to use alloys based on the primary aluminum (low Fe content, but high costs) or the secondary aluminum (high Fe content, but reasonable costs) for a cast product is a common problem. The main expected influence of higher iron content is to increase porosity and decrease mechanical and fatigue properties. Therefore, this work is focused on assessment of the higher Fe content influence on porosity and iron-rich intermetallic phases formation and, hence, changes in the mechanical properties, with simultaneously keeping the production economical. The quality of castings was measured by application of the 2D technology (image analysis) and the 3D technology (CT analysis), as well. Results show that technologies of assessment are comparable and length of the Fe-rich phases is not critical for mechanical properties, but it is important for porosity formation in materials with the higher amount of Fe.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Assessing time-of-flight signal-to-noise ratio gains within the myocardium and subsequent reductions in administered activity in cardiac PET studies

Background: Time-of-flight (TOF) is known to increase signal-to-noise ratio (SNR) and facilitate reductions in administered activity. Established measures of SNR gain are derived from areas of uniform uptake, which is not applicable to the heterogeneous uptake in cardiac PET images using fluoro-deoxyglucose (FDG). This study aimed to develop a technique to quantify SNR gains within the myocardium due to TOF. Methods: Reference TOF SNR gains were measured in 88 FDG oncology patients. Phantom data were used to translate reference SNR gains and validate a method of quantifying SNR gains within the myocardium from parametric images produced from multiple replicate images. This technique was applied to 13 FDG cardiac viability patients. Results: Reference TOF SNR gains of +23% ± 8.5% were measured in oncology patients. Measurements of SNR gain from the phantom data were in agreement and showed the parametric image technique to be sufficiently robust. SNR gains within the myocardium in the viability patients were +21% ± 2.8%. Conclusion: A method to quantify SNR gains from TOF within the myocardium has been developed and evaluated. SNR gains within the myocardium are comparable to those observed by established methods. This allows guidance for protocol optimization for TOF systems in cardiac PET.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2018

Investigation of dose reduction in cardiac perfusion SPECT via optimization and choice of the image reconstruction strategy

Background: We investigated the extent to which the administered dose (activity) level can be reduced without sacrificing diagnostic accuracy for three reconstruction strategies for SPECT-myocardial perfusion imaging (MPI). Methods: We optimized the parameters of the three reconstruction strategies for perfusion-defect detection over a range of simulated administered dose levels using a set of hybrid studies (derived from 190 subjects) consisting of clinical SPECT-MPI data modified to contain realistic simulated lesions. The optimized strategies we considered are filtered backprojection (FBP) with no correction for degradations, ordered-subsets expectation-maximization (OS-EM) with attenuation correction (AC), scatter correction (SC), and resolution correction (RC), and OS-EM with scatter and resolution correction only. Each study was evaluated using a total perfusion deficit (TPD) score computed by the Quantitative Perfusion SPECT (QPS) software package. We conducted a receiver operating characteristics (ROC) study based on the TPD scores for each dose level and reconstruction strategy. Results: For FBP, the achieved optimum values of the area under the ROC curve (AUC) at 100%, 50%, 25%, and 12.5% of standard dose were 0.75, 0.74, 0.72, and 0.70, respectively, compared to 0.81, 0.79, 0.76, and 0.74 for OS-EM with AC–SC–RC and 0.78, 0.77, 0.74, 0.72 for OS-EM with SC–RC. Conclusions: Our results suggest that studies reconstructed by OS-EM with AC–SC–RC could possibly be reduced, on average, to 25% of the originally administered dose without causing diagnostic accuracy (AUC) to decrease below that of FBP.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2019

A combined static-dynamic single-dose imaging protocol to compare quantitative dynamic SPECT with static conventional SPECT

Background: SPECT myocardial perfusion imaging (MPI) is a clinical mainstay that is typically performed with static imaging protocols and visually or semi-quantitatively assessed for perfusion defects based upon the relative intensity of myocardial regions. Dynamic cardiac SPECT presents a new imaging technique based on time-varying information of radiotracer distribution, which permits the evaluation of regional myocardial blood flow (MBF) and coronary flow reserve (CFR). In this work, a preliminary feasibility study was conducted in a small patient sample designed to implement a unique combined static-dynamic single-dose one-day visit imaging protocol to compare quantitative dynamic SPECT with static conventional SPECT for improving the diagnosis of coronary artery disease (CAD). Methods: Fifteen patients (11 males, four females, mean age 71 ± 9 years) were enrolled for a combined dynamic and static SPECT (Infinia Hawkeye 4, GE Healthcare) imaging protocol with a single dose of {sup 99m}Tc-tetrofosmin administered at rest and a single dose administered at stress in a one-day visit. Out of 15 patients, eleven had selective coronary angiography (SCA), 8 within 6 months and the rest within 24 months of SPECT imaging, without intervening symptoms or interventions. The extent and severity of perfusion defects in each myocardial region was graded visually. Dynamically acquired data were also used to estimate the MBF and CFR. Both visually graded images and estimated CFR were tested against SCA as a reference to evaluate the validity of the methods. Results: Overall, conventional static SPECT was normal in ten patients and abnormal in five patients, dynamic SPECT was normal in 12 patients and abnormal in three patients, and CFR from dynamic SPECT was normal in nine patients and abnormal in six patients. Among those 11 patients with SCA, conventional SPECT was normal in 5, 3 with documented CAD on SCA with an overall accuracy of 64%, sensitivity of 40% and specificity of 83%. Dynamic SPECT image analysis also produced a similar accuracy, sensitivity, and specificity. CFR was normal in 6, each with CAD on SCA with an overall accuracy of 91%, sensitivity of 80%, and specificity of 100%. The mean CFR was significantly lower for SCA detected abnormal than for normal patients (3.86±1.06 vs 1.94±0. 0.67, P < 0.001). Conclusions: The visually assessed image findings in static and dynamic SPECT are subjective, and may not reflect direct physiologic measures of coronary lesion based on SCA. The CFR measured with dynamic SPECT is fully objective, with better sensitivity and specificity, available only with the data generated from the dynamic SPECT method.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2019

Improving perfusion defect detection with respiratory motion correction in cardiac SPECT at standard and reduced doses

Background: In cardiac SPECT perfusion imaging, respiratory motion can cause non-uniform blurring in the reconstructed myocardium. We investigate the potential benefit of respiratory correction with respiratory-binned acquisitions, both at standard dose and at reduced dose, for defect detection and for left ventricular (LV) wall resolution. Methods: We applied two reconstruction methods for respiratory motion correction: post-reconstruction motion correction (PMC) and motion-compensated reconstruction (MCR), and compared with reconstruction without motion correction (Non-MC). We quantified the presence of perfusion defects in reconstructed images by using the total perfusion deficit (TPD) scores and conducted receiver-operating-characteristic (ROC) studies using TPD. We quantified the LV spatial resolution by using the FWHM of its cross-sectional intensity profile. Results: The values in the area-under-the-ROC-curve (AUC) achieved by MCR, PMC, and Non-MC at standard dose were 0.835, 0.830, and 0.798, respectively. Similar AUC improvements were also obtained by MCR and PMC over Non-MC at 50%, 25%, and 12.5% of full dose. Improvements in LV resolution were also observed with motion correction. Conclusions: Respiratory-binned acquisitions can improve perfusion-defect detection accuracy over traditional reconstruction both at standard dose and at reduced dose. Motion correction may contribute to achieving further dose reduction while maintaining the diagnostic accuracy of traditional acquisitions. [French] French Abstract: Contexte: Les mouvements respiratoires peuvent entrainer des artefacts de uniformité lors de la reconstruction des images de perfusion myocardique en SPECT. Dans cet article, nous rapportons nos résultats sur le bénéfice potentiel du « gating » respiratoire avec des doses standards et réduites de radio-pharmaceutiques pour la détection des anomalies de perfusion et les mesures de la paroi ventriculaire gauche. Méthodes: Nous avons appliqué deux méthodes de reconstruction pour la correction du mouvement respiratoire: la première fait appel a une correction après reconstruction des images (PMC) ; la seconde fait appel à la correction des images avant reconstruction (MRC). Les deux approches ont été comparées à la reconstruction sans correction de mouvement (Non-MC). Nous avons quantifié les déficits de perfusion myocardiques sur les images reconstruites avec le système des scores de déficit de perfusion et analysé les résultats en utilisant les courbes ROC. Nous avons quantifié la résolution spatiale du VG en utilisant le FWHM du profil d’intensité de sa section transversale. Résultats: Les valeurs des surfaces en dessous des courbes ROC (AUC) obtenues par MCR, PMC et Non-MC avec doses standard de radio-pharmaceutiques étaient de 0,835, 0,830 et 0,798, respectivement. Des améliorations similaires de l’AUC ont également été obtenues par MCR et PMC sur Non-MC avec 50%, 25% et 12,5% des doses entières. Les mesures de résolution spatiale de la paroi du VG ont également été améliorées avec la correction des mouvements respiratoires. Conclusions: La correction des images de perfusion myocardiques en SPECT par « gating » respiratoire paraît améliorer la quantification des déficits perfusionels à la fois à dose standard et à dose réduite de radio-pharmaceutiques. L’application de cette correction devrait permettre de réduire les doses de radio-pharmaceutiques utilisées tout en maintenant la précision diagnostique des acquisitions traditionnelles. [Spanish] Spanish Abstract: Antecedentes: En los estudios de perfusión cardiaca por SPECT, los movimientos respiratorios pueden causar distorsión no uniforme en el miocardio reconstruido. Investigamos el beneficio potencial de la corrección respiratoria con adquisición de imágenes sincronizadas con la respiración, tanto a dosis estándar como a dosis reducida, para detección de defectos y para resolución de pared de ventrículo izquierdo (VI). Métodos: Aplicamos dos métodos de reconstrucción para corrección de movimientos respiratorios: Corrección de movimiento post reconstrucción (PMC) y reconstrucción compensada a movimiento (MCR), y los comparamos con la reconstrucción sin corrección de movimiento (Non-MC). Cuantificamos la presencia de defectos de perfusión en las imágenes reconstruidas usando los scores de déficit total de perfusión (TPD) y análisis ROC usando el TPD. Cuantificamos la resolución espacial del VI usando la anchura a media altura de su perfil de intensidad transversal. Resultados: Los valores en el área bajo la curva ROC (ABC) obtenidos por MCR, PMC y Non-MC a dosis estándar fueron 0.835, 0.830 y 0.798, respectivamente. Mejorías similares del ABC también se obtuvieron por MCR y PMC, sobre Non-MC a 50%, 25% y 12.5% de la dosis completa. Las mejorías en la resolución del VI fueron observadas también con corrección del movimiento. Conclusiones: Las adquisiciones sincronizadas con la respiración pueden mejorar la precisión de la detección de defectos de perfusión sobre las reconstrucciones tradicionales tanto a dosis estándar como a dosis reducida. La corrección de movimiento puede contribuir a lograr mayor reducción de la dosis manteniendo la precisión diagnóstica de las adquisiciones tradicionales. [Chinese] Chinese Abstract: 背景: 在心脏 SPECT 灌注成像中, 呼吸运动会导致心肌重建的不均匀模糊。我们研究了无论是标准剂量还是减少剂量的情况下, 呼吸跟踪采集的呼吸校正用于图像缺损检测和左心室 (LV) 室壁分辨率的潜在益处。 方法: 我们使用了两种呼吸运动校正的重建方法:重建后运动校正 (PMC) 和运动补偿重建 (MCR), 并与没有运动校正的重建 (Non-MC) 进行比较。 通过总灌注缺损 (TPD) 评分和其接受者操作特性曲线 (ROC) 来量化重建图像中的灌注缺陷。通过LV横截面强度分布的 FWHM来量化 LV 空间分辨率。 结果: MCR, PMC 和 Non-MC 在标准剂量下所获得的 ROC 曲线下面积 (AUC) 的值分别为0.835, 0.830 和 0.798。 在全剂量下, MCR, PMC和 Non-MC也获得类似的 AUC 提高, 分别为 50%, 25% 和 12.5%。 在运动校正下, LV的分辨率也得到了改善。 结论: 在标准剂量和减少剂量的情况下, 呼吸跟踪采集可以改善灌注缺损检测的准确性。 运动校正可能有助于进一步实现减少剂量的目标, 同时保证通过传统检测方法的诊断准确性。.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2019

How do we establish cardiac sympathetic nervous system imaging with {sup 123}I-mIBG in clinical practice? Perspectives and lessons from Japan and the US

Cardiac denervation is associated with progressive left ventricular (LV) dysfunction, ventricular arrhythmias, and sudden cardiac death (SCD) in heart failure (HF). In this regard, it is important to evaluate cardiac-specific sympathetic nervous system (SNS) function. The radiotracer Iodine-123 meta-iodobenzylguanidine ({sup 123}I-mIBG) can noninvasively evaluate pre-synaptic SNS function. Recent multicenter trials have shown {sup 123}I-mIBG to have strong predictive value for fatal arrhythmias and cardiac death in HF. {sup 123}I-mIBG was initially developed in the USA in the 1970s. In 1992, the Japanese Ministry of Health and Labour approved {sup 123}I-mIBG for the assessment of cardiac function. Following approval, the Japanese nuclear cardiology community developed {sup 123}I-mIBG imaging services in various medical centers. Japanese groups have been trying to establish the clinical utility of {sup 123}I-mIBG and standardize parameters for data acquisition and image analysis. The US Food and Drug Administration (FDA) has approved clinical use of {sup 123}I-mIBG for cardiac and non-cardiac imaging. However, clinical use of {sup 123}I-mIBG in the US has been very limited. The number of {sup 123}I-mIBG studies in Japan has also been limited. There are similarities and differences between the two countries. To establish the clinical utility of {sup 123}I-mIBG in both countries, it is important to characterize the situations of {sup 123}I-mIBG in each.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2019

No need for frame-wise attenuation correction in dynamic Rubidium-82 PET for myocardial blood flow quantification

Background: Regadenoson-induced stress causes a repositioning of the heart, myocardial creep, in half of the patients undergoing Rubidium-82 (Rb-82) positron emission tomography (PET). As a result, misalignment of dynamic PET and computer tomography (CT) may occur, possibly affecting CT-based attenuation correction (AC) and thereby PET-based myocardial blood flow (MBF) quantification. Our aim was to determine the need for frame-wise PET-CT AC to obtain reliable MBF measurements. Methods: 31 Out of 64 consecutive patients had myocardial creep during regadenoson-induced stress Rb-82 PET-CT and were included. Prior to PET image reconstruction, we applied two AC methods; single PET-CT alignment and frame-wise alignment in which PET time-frames with myocardial creep were individually co-registered with CT. The PET-CT misalignment was then quantified and MBFs for the three vascular territories and whole myocardium were calculated and compared between both methods. Results: The magnitude of misalignment due to myocardial creep was 13.8 ± 4.5 mm in caudal-cranial direction, 1.8 ± 2.1 mm in medial-lateral and 2.5 ± 1.8 mm in anterior-posterior direction. Frame-wise PET-CT registration did not result in different MBF measurements (P ≥ .07) and the magnitude of misalignment and MBF differences did not correlate (P ≥ .58). Conclusion: There is no need for frame-wise AC in dynamic Rb-82 PET for MBF quantification. Single alignment seems sufficient in patients with myocardial creep.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2019

Selection of abstracts from the scientific sessions of The Society Of Nuclear Medicine and Molecular Imaging annual meeting Anaheim CA

This mini-review highlights cardiovascular studies that were presented during the Society of Nuclear Medicine and Molecular Imaging (SNMMI) 2019 annual meeting in Anaheim, California. The aim is to provide the readers insight to noteworthy studies related to the fields of nuclear cardiology presented during the conference. Although cardiovascular applications of positron emission tomography (PET) and single-photon emission computed tomography (SPECT) are not the primary focus of the SNMMI, several scientific teams working in this field presented their latest findings in Anaheim. While this review is directed to the benefit of those who were not able to attend the annual meeting, we believe that a general overview may also be useful for those who did attend as it is often difficult to get exposure to all the high-quality abstracts presented at this large conference.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2019

Leveraging latest computer science tools to advance nuclear cardiology

Nuclear cardiology has unique advantages compared to other modalities, since the image analysis is already much more automated compared to what is currently clinically performed for CT, MR, or echocardiography imaging. The diverse image and clinical data available to assess coronary disease function, perfusion, flow, and associated CT data provide new opportunities, but logistically these additional assessments increase the overall complexity of SPECT/PET reporting, necessitating additional expertise and time. The advances in artificial intelligence software can be leveraged to obtain comprehensive risk predictions and diagnoses from all available data. They will allow nuclear cardiology to retain competitive edge compared to other modalities and improve its overall clinical utility. These tools will enhance diagnosis and risk prediction beyond what is possible by subjective visual analysis and mental integration of data by physicians.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2018

MSiReader v1.0: Evolving Open-Source Mass Spectrometry Imaging Software for Targeted and Untargeted Analyses

A major update to the mass spectrometry imaging (MSI) software MSiReader is presented, offering a multitude of newly added features critical to MSI analyses. MSiReader is a free, open-source, and vendor-neutral software written in the MATLAB platform and is capable of analyzing most common MSI data formats. A standalone version of the software, which does not require a MATLAB license, is also distributed. The newly incorporated data analysis features expand the utility of MSiReader beyond simple visualization of molecular distributions. The MSiQuantification tool allows researchers to calculate absolute concentrations from quantification MSI experiments exclusively through MSiReader software, significantly reducing data analysis time. An image overlay feature allows the incorporation of complementary imaging modalities to be displayed with the MSI data. A polarity filter has also been incorporated into the data loading step, allowing the facile analysis of polarity switching experiments without the need for data parsing prior to loading the data file into MSiReader. A quality assurance feature to generate a mass measurement accuracy (MMA) heatmap for an analyte of interest has also been added to allow for the investigation of MMA across the imaging experiment. Most importantly, as new features have been added performance has not degraded, in fact it has been dramatically improved. These new tools and the improvements to the performance in MSiReader v1.0 enable the MSI community to evaluate their data in greater depth and in less time. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2019

The Influence of MS Imaging Parameters on UV-MALDI Desorption and Ion Yield

Ultraviolet matrix-assisted laser desorption/ionization mass spectrometry imaging (UV-MALDI MSI) is a widely used technique for imaging molecular distributions within biological systems. While much work exists concerning desorption in UV-MALDI MS, the effects of commonly varied parameters for imaging applications (repetition rate, use of continuous raster mode and raster speed), which determine spatial resolution and limits of detection for the technique, remain largely unknown. We use multiple surface characterization modalities to obtain quantitative measurements of material desorption and analyte ion yield in thin film model systems of two matrix compounds, arising from different UV-MALDI MSI sampling conditions. Observed changes in resulting ablation feature point to matrix-dependent spatial resolution and laser-induced matrix modification effects. Analyte ion yields of 10{sup −9} to 10{sup −6} are observed. Complex changes in ion yield, between spot and raster sampling and arising from varied laser repetition rate and raster speed, are observed. .

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2019

Screening of the Suzuki Cross-Coupling Reaction Using Desorption Electrospray Ionization in High-Throughput and in Leidenfrost Droplet Experiments

Suzuki cross-coupling is a widely performed reaction, typically using metal catalysts under heated conditions. Acceleration of the Suzuki cross-coupling reaction has been previously explored in microdroplets using desorption electrospray ionization mass spectrometry (DESI-MS). Building upon previous work, presented here is the use of a high-throughput DESI-MS screening system to identify optimal reaction conditions. Multiple reagents, bases, and stoichiometries were screened using the automated system at rates that approach 10,000 reaction mixture systems per hour. The DESI-MS system utilizes reaction acceleration in microdroplets to allow rapid screening. The results of screening of an array of reaction mixtures using this technique are presented as product ion images via standard MS imaging software, facilitating quick readout. Instructive comparisons are provided with another method of generating droplets for reaction acceleration—the Leidenfrost technique. Acceleration factors greater than 200 were measured for brominated substrates, paralleling the DESI-MS results. Acceleration factors dropped to near unity with highly substituted pyridines, attributable to a steric effect. The reaction proceeded in the absence of a base in Leidenfrost droplets although no product formation was seen without base in the bulk or in the DESI-MS screening experiments. These differences between Leidenfrost chemistry and the bulk and in droplets formed in high-throughput DESI are tentatively attributed to extremes of pH associated with the surfaces of Leidenfrost droplets. .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗