- 标题
- 摘要
- 关键词
- 实验方案
- 产品
-
Laser Desorption Ionization-Mass Spectrometry of Linear Diphenylenes Encapsulated in Crystalline Sponge
摘要： Three linear diphenylene compounds having one, two, and three double bonds, respectively, were encapsulated in a nano-porous coordination complex called “crystalline sponge” (CS). The presence of these diphenylene compounds in CS was confirmed by single-crystal X-ray structure analysis and NMR spectroscopy. In CS, CH-π and π-π interactions between the pyridyl group of the triazine ligand in the CS framework and the phenyl group of the diphenylene compounds were determined on the basis of the geometrical orientation in the nanopore. After the single-crystal X-ray structure analysis, the same single crystal was subjected to imaging mass spectrometry (IMS). Molecular ion peaks were almost equally detected in all regions of the target plate where the CSs were present and the search for hotspots was no longer necessary. At the same time, ion peaks derived from the triazine ligand and its metal complex, which are components of the CS framework, were clearly observed. CSs have been shown to be one of the effective matrixes for laser desorption ionization of trace linear conjugate compounds.
关键词： crystalline sponge,diphenylene compound,imaging mass spectrometry
更新于2025-09-23 15:21:01
-
Low temperature platinum chemical vapor deposition on functionalized self-assembled monolayers
摘要： The reaction pathways of Pt CVD using (COD)PtMe2 – xClx (x = 0, 1, 2) have been investigated on functionalized self-assembled monolayers (SAMs) as models for organic substrates. Residual gas analysis for (COD)PtMe2 and (COD)PtMeCl is consistent with the loss of methyl radicals as the initial step in deposition, while for (COD)PtCl2, the first step is the loss of a chlorine radical. It is further shown using x-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry that the deposition process leads to chemical damage of the SAM layer and little Pt deposition. Using this understanding, it is demonstrated that the Pt CVD rate can be controlled using a radical trap. In the presence of 1,4-cyclohexadiene, a well-known alkyl radical trap, Pt deposition was increased by 5× to 10×, creating a room-temperature effective Pt CVD process.
关键词： time-of-flight secondary ion mass spectrometry,x-ray photoelectron spectroscopy,Pt CVD,chemical vapor deposition,self-assembled monolayers,radical trap
更新于2025-09-23 15:21:01
-
Comparison of quantitative analyses using SIMS, atom probe tomography, and femtosecond laser ablation inductively coupled plasma mass spectrometry with Si <sub/>1a??X</sub> Ge <sub/>X</sub> and Fe <sub/>1a??X</sub> Ni <sub/>X</sub> binary alloys
摘要： Due to their electrical and physical properties, Si1?XGeX materials are widely used in microelectronic devices. In particular, the Ge component found within Si1?XGeX compounds is important for enhancing carrier mobility and altering the lattice constant of metal-oxide-semiconductor field-effect transistors. In this study, magnetic sector secondary ion mass spectrometry (magnetic sector SIMS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were used to determine the accurate concentrations of major compositions present within binary alloy samples. However, quantitative SIMS analysis is limited by the matrix effect, which influences the sputter yield of an element in a compound and alters the secondary ionization yields. Quantitative deviations that were due to the matrix effect were reduced by using Cs cluster ions (MCs+ and MCs2+) instead of elemental ions; the SIMS results using the elements were, therefore, compared with those using MCs+ and MCs2+ cluster ions. In the case of Fe1?XNiX alloys that have a less matrix effect compared to Si1?XGeX alloys, both the Cs primary ion beam (Cs+) and an oxygen primary ion beam (O2+) were used to measure the Fe1?XNiX compositions. The quantitative results from the two different primary ion beams were then compared to understand the ionization process. Deviations in the quantitative values gained with the O2+ beam were lower than those obtained using the Cs+ primary ions, meaning that using oxygen as the primary ion improves the accuracy in quantifying Fe1?XNiX compounds. Other reliable tools for analysis such as atom probe tomography and femtosecond laser ablation inductively coupled plasma mass spectrometry were also used in the quantitative analysis, with results that were consistent with the most accurate results obtained using magnetic sector SIMS and ToF-SIMS.
关键词： Si1?XGeX,femtosecond laser ablation inductively coupled plasma mass spectrometry,atom probe tomography,SIMS,Fe1?XNiX,binary alloys
更新于2025-09-23 15:21:01
-
Laser-Induced Dissociation of the Monolayer of Adsorbed Methanol Molecules
摘要： Astronomical observations indicate a high abundance of methanol molecules in the gas phase of molecular-cloud dense cores, which cannot be explained by gas-phase chemical reactions only. A significant contribution to the methanol abundance should be provided by chemical reactions on the dust particle surface with subsequent desorption of the produced molecules into the gas phase. For the development and refinement of models involving these processes, laboratory studies of photo-induced processes occurring in the adsorbed material are necessary. In this paper, the experiment results of adsorbed methanol molecules are presented. A methanol molecule monolayer, physically adsorbed on fused silica surface cooled by liquid nitrogen (Т ～ 100 K), was irradiated in high vacuum by nanosecond pulses of an excimer KrF laser with a fixed wavelength λ = 248 nm. The photodissociation products of three-photon laser excitation were recorded by a quadrupole mass spectrometer. Relative yields of photofragments H, OH, and CH3 were determined. Photolysis of partially deuterated CH3OH molecules has shown that hydrogen atoms can be ejected both from hydroxyl and methyl groups. In contrast to the isolated molecule photolysis in the gas phase and dissociation of the multilayer molecular coatings, photoexcitation of adsorbed methanol monolayer even in the energy region of 10 eV does not cause noticeable chemical transformations and does not lead to the formation of molecular components H2 and CH4. Due to existing astrochemical modeling problems, possible application methods of the obtained laboratory results are considered.
关键词： chemical reactions,astronomical observations,adsorbed monolayer,mass spectrometry,photo-induced processes,gas phase,dust particle surface,KrF laser,photodissociation,methanol
更新于2025-09-23 15:21:01
-
Fundamental understanding of chemical processes in extreme ultraviolet resist materials
摘要： New photoresists are needed to advance extreme ultraviolet (EUV) lithography. The tailored design of efficient photoresists is enabled by a fundamental understanding of EUV induced chemistry. Processes that occur in the resist film after absorption of an EUV photon are discussed, and a new approach to study these processes on a fundamental level is described. The processes of photoabsorption, electron emission, and molecular fragmentation were studied experimentally in the gas-phase on analogs of the monomer units employed in chemically amplified EUV resists. To demonstrate the dependence of the EUV absorption cross section on selective light harvesting substituents, halogenated methylphenols were characterized employing the following techniques. Photoelectron spectroscopy was utilized to investigate kinetic energies and yield of electrons emitted by a molecule. The emission of Auger electrons was detected following photoionization in the case of iodo-methylphenol. Mass-spectrometry was used to deduce the molecular fragmentation pathways following electron emission and atomic relaxation. To gain insight on the interaction of emitted electrons with neutral molecules in a condensed film, the fragmentation pattern of neutral gas-phase molecules, interacting with an electron beam, was studied and observed to be similar to EUV photon fragmentation. Below the ionization threshold, electrons were confirmed to dissociate iodo-methylphenol by resonant electron attachment.
关键词： photoabsorption,molecular fragmentation,electron emission,photoresists,mass-spectrometry,Auger electrons,photoelectron spectroscopy,EUV lithography,resonant electron attachment,halogenated methylphenols
更新于2025-09-23 15:21:01
-
Preparation and comparison of Fe3O4@graphene oxide nanoclusters for analysis of glimepiride in urine by surface-assisted laser desorption/ionization time-of-flight mass spectrometry
摘要： Graphene oxide (GO) has the ability to absorb certain compounds, and it can be modified with functional groups for different purposes; for instance, iron oxide (IO) nanoparticles can be used to concentrate analyte by a magnet. Recently, many kinds of GO have been developed, such as single-layer GO (SLGO), two-to-four layers of GO (i.e., few-layer GO, FLGO2–4), and four-to-eight layers of GO (i.e., multi-layer GO, MLGO4–8). However, the abilities of these layered GO coated with IO nanoparticles have not been investigated. In this study, we conducted a novel analysis of glimepiride by using layered GO-coated magnetic clusters of IO nanoparticles that were synthesized through a simple and facile emulsion-solvent evaporation method. The methodology is based on (i) enrichment of glimepiride using the layered GO-coated magnetic clusters of IO nanoparticles (IO@SLGO, IO@FLGO2–4, and IO@MLGO4–8), and (ii) rapid determination using magnetic cluster–based surface-assisted laser desorption/ionization time-of-flight mass spectrometry (SALDI-TOFMS). We found that IO@MLGO4–8, the magnetic cluster with the greatest number of GO layers, had the best limit of detection (28.6 pmol/μL for glimepiride). The number of GO layers played a significant role in increasing the sensitivity of the SALDI-MS, indicating that the size of GO in the magnetic clusters contributed to the desorption/ionization efficiency. To the best of our knowledge, this is the first study to enrich glimepiride using magnetic clusters of different GO types and to show that the glimepiride in HLB purified urine adsorbed by magnetic clusters can be analyzed by SALDI-TOFMS.
关键词： Mass spectrometry,Iron oxide,Glimepiride,Nanocluster,SALDI,Graphene oxide
更新于2025-09-23 15:21:01
-
Simulation studies of the laser ablation ion source at the SHIPTRAP setup
摘要： A gas-filled miniature Radio-Frequency Quadrupole (mini-RFQ) was recently implemented into the SHIPTRAP laser ablation ion source to thermalize the laser-ablated ions and thus improve production efficiency as well as sample preparation. This source provides reference ions of various elements for online experiments with the SHIPTRAP mass spectrometer. In addition, it can be used to provide long-lived rare and radioactive isotopes available only in small sample sizes for high-precision mass measurements or to study systematic uncertainties. The performance of the laser ablation ion source was simulated using the COMSOL Multiphysics modeling software package. These studies indicate that a revised mechanical geometry and an optimized RF field improve the performance significantly.
关键词： Penning traps,Surface ionization ion source,Mass spectrometry,Laser ablation ion source
更新于2025-09-23 15:21:01
-
Highly selective two-step laser ionization schemes for the analysis of actinide mixtures
摘要： Resonance ionization mass spectroscopy has proven to be a very efficient and selective method for the spatially resolved ultratrace determination of actinide contaminations, and the analysis of specific element and isotopic distributions on surfaces and environment particles. We report on the identification of highly element-selective optical excitation schemes identified for this purpose, with a particular focus on the precise determination of the isobaric ratios of 235U to 239Pu as well as 243Am to 241Pu. The chosen two-step ionization schemes were characterized with respect to their element selectivity on synthetic multi-element actinide mixtures, with an element ratio Pu : Am : U of 1 : 10 : 104, a composition which is typical, e.g., for spent nuclear reactor fuels.
关键词： Mass spectrometry,Actinides,Laser spectroscopy,Multi-element mixture,Isotope ratio
更新于2025-09-23 15:21:01
-
Raman spectroscopy coupled with ambient ionization mass spectrometry: A forensic laboratory investigation into rapid and simple dual instrumental analysis techniques
摘要： We present a laboratory experiment, developed around a pair of instrumental analysis techniques, Raman spectroscopy and ambient ionization mass spectrometry (MS), conducted by senior chemistry undergraduate students for bulk analysis of over-the-counter drugs using benchtop versions of the two instruments, as well as trace analysis of illicit drugs utilizing the corresponding portable instruments. The identification and confirmation of seized drugs is a routine operation in forensic laboratories that can be simplified using these two instrumental techniques in tandem. Bulk samples are readily analyzed using conventional Raman spectroscopy followed by paper cone spray ionization (PCSI) MS, while trace analysis is allowed by a simple single-substrate dual-analyzer method using surface enhanced Raman spectroscopy (SERS) from paper followed by paper spray ionization (PSI) MS. The introduction of these novel strategies to the students exposed them to potential career paths in forensic science by means of a hands-on experience that provided fundamental knowledge about this set of analytical methods, including intercomparisons of their performance, as well as practical issues like costs, regulations and databases. The use of portable instrumentation represents an additional learning experience for the students, considering that it is cutting-edge technology that is just now being transferred from academic to industrial labs and that it allows a valuable discussion of the advantages and disadvantages of bringing the laboratory to the field.
关键词： Mass spectrometry,Hands-on learning,Forensic analysis,Drugs of abuse,Paper cone spray ionization,Paper spray ionization,Paper surface enhanced Raman spectroscopy,Raman spectroscopy,Ambient ionization,Laboratory instruction
更新于2025-09-23 15:21:01
-
High-Throughput Fingerprinting of Rhizobial Free Fatty Acids by Chemical Thin-Film Deposition and Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry
摘要： Fatty acids (FAs) represent an important class of metabolites, impacting on membrane building blocks and signaling compounds in cellular regulatory networks. In nature, prokaryotes are characterized with the most impressing FA structural diversity and the highest relative content of free fatty acids (FFAs). In this context, nitrogen-fixing bacteria (order Rhizobiales), the symbionts of legumes, are particularly interesting. Indeed, the FA profiles influence the structure of rhizobial nodulation factors, required for successful infection of plant root. Although FA patterns can be assessed by gas chromatography—(GC-) and liquid chromatography—mass spectrometry (LC-MS), sample preparation for these methods is time-consuming and quantification suffers from compromised sensitivity, low stability of derivatives and artifacts. In contrast, matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF-MS) represents an excellent platform for high-efficient metabolite fingerprinting, also applicable to FFAs. Therefore, here we propose a simple and straightforward protocol for high-throughput relative quantification of FFAs in rhizobia by combination of Langmuir technology and MALDI-TOF-MS featuring a high sensitivity, accuracy and precision of quantification. We describe a step-by-step procedure comprising rhizobia culturing, pre-cleaning, extraction, sample preparation, mass spectrometric analysis, data processing and post-processing. As a case study, a comparison of the FFA metabolomes of two rhizobia species—Rhizobium leguminosarum and Sinorhizobium meliloti, demonstrates the analytical potential of the protocol.
关键词： bacteria,metabolic fingerprinting,matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF-MS),barium monocarboxylates,free fatty acids (FFAs),chemical deposition technique,Langmuir film technology,rhizobia
更新于2025-09-23 15:21:01