四极质谱计在真空检漏中的应用

介绍了使用四极质谱计进行真空检漏的原理和方法,分别对超高和极高真空系统做了检漏实验研究，并取到了满意的结果。四极质谱计检漏有检漏仪检漏无法比拟的优点，适合在真空工程中推广应用。     

ESI离子阱质谱仪真空系统设计

自主研发质谱仪并能够将其产业化生产是一项十分有意义的工作.质谱仪的工作原理决定了其核心部件(质量分析器和检测器)需要在真空下工作,因此质谱仪的真空系统设计是质谱仪研发工作的基础.本文针对ESI离子阱质谱仪科研样机进行真空系统设计.     

The calibration of Bonner sphere spectrometer

Bonner sphere spectrometer (BSS) is used in radiation protection measurement because of its wide energy range (thermal to MeV) and easy operation. Mitsubishi Heavy Industries (MHI) has used BSS to obtain neutron spectrum and has used the neutron spectrum to estimate neutron dose or induced activity. Calibration of BSS is important to estimate precise neutron dose or induced activity. MHI BSS was calibrated at National Institute of Advanced Industrial Science and Technology (AIST). The calibration results at AIST are in good agreement with calculation results.     

Teflon feedthrough for coupling optical fibers into ultrahigh vacuum systems

We present an inexpensive, reusable method of introducing optical fibers into ultrahigh vacuum systems. A Teflon ferrule with a center-drilled hole slightly larger than the fiber diameter replaces the metal ferrules of a standard Swagelok connector. The Swagelok connector when tightened compresses the Teflon to form a vacuum seal for pressures of 相似文献   

四极质谱计工作参数对校准因子影响研究

介绍了在危险气体成份分析系统校准装置上,开展四极质谱计工作参数对校准因子影响的实验研究工作。在实验中,每次改变四极质谱计的一个工作参数,如电子能量、离子能量、发射电流、分辨本领、扫描速度、收集方式等,测量氮谱峰离子流强度和被校气体谱峰离子流强度,利用校准因子计算公式,通过计算获得校准因子值,并分析校准因子的变化趋势,给出四极质谱计实验室校准参数设置,减小校准不确定度。     

Pulsed oscillating mass spectrometer: a miniaturized type of time-of-flight mass spectrometer

We report the development, characterization, and performance of a new type of time-of-flight mass analyzer that employs an oscillatory ion flight path and uses secondary electrons to record the mass spectrum. The analyzer is simple in concept and design and inexpensive to build and has been made as small as 6-cm total length. The oscillating ions produce a periodic secondary electron signal whose frequency is mass dependent in mathematically the same way as a conventional time-of-flight analyzer. Because of the oscillating nature of the ions, we have called the analyzer the pulsed oscillating mass spectrometer.     

The flight of macromolecular complexes in a mass spectrometer

The discovery that conditions can be found such that non-covalent macromolecular complexes can survive the transition from solution to gas phase and remain intact during their flight in a mass spectrometer is an intriguing observation. While the nature of the interaction between the components, either ionic, hydrophobic or van der Waals, undoubtedly has an effect on the stability of these gas phase species, the role of small molecules in conferring additional stability is often overlooked. Here we review historical aspects of the development of mass spectrometry for macromolecular complexes with particular focus on the role of small molecules in stabilizing gas-phase complexes. Moreover, we demonstrate how the dissociation of small molecules from subunits within a macromolecular complex can be used to probe the topological arrangement. Overall, therefore, we show that mass spectrometry used in this way is capable of addressing features of the energy landscape not readily accessed by traditional structural biology approaches.     

Temporal sensitivity of the wavelength calibration of a photodiode array spectrometer

Subtle differences in the relationship between wavelength and pixel on photodiode array spectrometers contribute to difficulties in transferring calibrations from one instrument to another and may even introduce errors on a single instrument over time. To quantify the level of drift that might be expected in photodiode instruments, we calibrated the wavelength scale of two Zeiss MMS-1 photodiode spectrometers weekly over a 12-month period. We found no evidence of drift in the wavelength calibration. The wavelength calibration was consistent within 0.03 nm over at least 150 days and better than 0.1 nm over the year. To provide context for the wavelength accuracy, we applied small perturbations to wavelength in two partial least squares (PLS) models. We found that wavelength perturbations introduced a linear increase in bias of about 7%/nm (for example, a 1-nm perturbation shifted fruit dry matter prediction from 14% to 21%) in a kiwifruit dry-matter model and about 3.6 °C/nm in an Intralipid temperature model. By including small wavelength perturbations in the training sets, we were able to reduce this error to less than 1.7%/nm and 0.2 °C/nm in the dry-matter and temperature models, respectively. These results suggest that the wavelength scale of photodiode instruments can be very stable. However, in light of the high sensitivity of the PLS models we examined, we recommend testing and, where possible, mitigating the sensitivity of PLS models to small wavelength shifts.     

Gas desorption from a stainless-steel surface in ultrahigh vacuum devices

Degassing of stainless-steel surface in a vacuum system with high unit pumping speed was investigated. Possibility of efficient surface outgassing at 400 K has been confirmed. An attempt to describe phenomena connected with hydrogen desorption from surface at 300 K is presented.     

Ozonation of trifluralin particles: An experimental investigation with a vacuum ultraviolet photoionization aerosol time-of-flight mass spectrometer

The ozonation of trifluralin coated on azelaic acid particles is investigated with a vacuum ultraviolet photoionization aerosol time-of-flight mass spectrometer. The suspended trifluralin particles with the mean diameter of 270 nm react with 100 ppm ozone in an aerosol reaction chamber under ambient pressure and room temperature (1 atm, 298 K). The time-of-flight mass spectra of the trifluralin particles and the solid state ozonides are obtained. The assignments of the mass spectra reveal that the major primary ozonides of trifluralin particles are 2,6-dinitro-N-propyl-N-propanoyl-4-(trifluoromethyl) benzamine and 2,6-dinitro-N-(propan-2(and 3)-ol)-N-propyl-4-(trifluoromethyl) benzamine. The major secondary ozonides of trifluralin 2-ethyl-7-nitro-5-(trifluoromethyl) benzimidazole-3-oxide, 2,6-dinitro-N-propyl-4-(trifluoromethyl) benzenamine and 2,6-dinitro-N-(formyl)-N-propyl-4-(trifluoromethyl) benzamine are observed. The primary ozonides are directly resulted from the oxidation of N-propyl groups. The pathways of the primary ozonation are proposed in the paper.     

Optical measurements of ion trajectories through the vacuum interface of an inductively coupled plasma mass spectrometer

A flexible laser excited fluorescence system has been used to trace ion trajectories in the first vacuum stage of an inductively coupled plasma mass spectrometer. The system has been used to record the spatial distributions of ions immediately upstream from the sampling cone and in the 10 mm downstream from the cone for a variety of positions of the plasma with respect to the sampling cone. The data were used in turn to test the efficacy of scanning the plasma across the sampling cone to generate maps of ion distributions in the plasma. The maps generated by scanning the plasma across the cone are close approximations of the ion distribution immediately upstream from the sampling cone, but are not representative of distributions in an unperturbed plasma.     

The calibration of coaxial reflectometers using extension cables

It is shown that coaxial reflectometers, calibrated by a set of standards having a single type of connection, can be used to measure the reflections of remote devices with other types of connections.Translated from Izmeritelnaya Tekhnika, No. 10, pp. 47–48, October, 2004.     

Tuning of an electrospray ionization source for maximum peptide-ion transmission into a mass spectrometer

We describe assembly and optimization of a continuous flow nanoelectrospray source for high-performance analysis on a routine basis. It is derived from an inJection adaptable Fine Ionization Source ("JaFIS"), previously shown to be durable and easy to use (Geromanos, S.; et al. Rapid Commun. Mass Spectrom. 1998, 12, 551-556) and now modified for maximum sensitivity. Proper design, manufacturing, and quality control of spray needles with specific orifice diameters, in combination with precisely controlled helium backpressure and applied voltage, enable stable flows at 1-2 nL/min. Needle positioning and ion spray potential are hereby exceedingly important, as shifts by 0.5 mm or 25 V, respectively, cause significant reduction in signal strength. In addition to prolonged analysis times, ultralow flows also yield higher sensitivity, the result of an improved "overall ion transfer efficiency" measured to be approximately 5% at 1.6 nL/min. Used in combination with a "microtip" (Erdjument-Bromage, H.; et al. J. Chromatogr. A 1998, 826, 167-181), the optimized JaFIS implements infusion-style ESI-MS at sensitivities approaching capillary LC-MS. Spraying times in excess of 20 h allow for any number of tandem mass spectrometric analysis routines to be performed, and to average thousands of scans in every experiment, thereby further improving sensitivity. This was fully illustrated by extensive analysis of a 2-fmol peptide mixture, in a 2-microL volume, using a multimode MS approach.     

The electron-stimulated desorption ions from the ionizer of a quadrupole mass spectrometer

The species and the pressure dependence of the electron-stimulated desorption (ESD) ions from the grid surface of the ionizer of the quadrupole mass spectrometer were measured by the QMS with the Bessel-box-type energy analyzer (BB-QMS). The BB-QMS was developed in order to measure true mass spectra of gas phase without ESD ion effect in high to extreme high vacuum. The ESD ions observed in typical residual gasses such as water, carbon monooxide, oxygen and carbon dioxide were H⁺ (H₂O), O⁺ (H₂O, CO, O₂, CO₂), OH⁺ (H₂O). The intensity of the ESD ion signals showed saturation upon increasing coverage of the water molecules on the grid surface.     

In-source decay and pseudo tandem mass spectrometry fragmentation processes of entire high mass proteins on a hybrid vacuum matrix-assisted laser desorption ionization-quadrupole ion-trap time-of-flight mass spectrometer

In-source decay (ISD), although a process known for decades in mass spectrometry, has a renewed interest due to increased theoretical knowledge in fragmentation processes of large biomolecules coupled with technological improvements. We report here an original method consisting of isolating matrix-assisted laser desorption ionization (MALDI)-generated in-source fragments of large proteins and subsequently performing selective fragmentation experiments (up to four cycles) using a hybrid MALDI quadrupole ion-trap time-of-flight mass spectrometer (MALDI-QIT-TOF). This technology takes advantage of keeping high resolution on the selection of precursors and detection of fragments. It allows exhaustive N- and C-terminal sequencing of proteins. In this work, human serum albumin (HSA), β-casein, and recombinant Tau proteins were submitted to in source decay in the MALDI source. The fragments were stored in the ion-trap and submitted to sequential collision-induced dissociation (CID). Finally, ISD and pseudo MS(n) were performed on oxidized Tau protein and acetylated bovine serum albumin to identify amino acid modifications. This work highlights the potential of the MALDI-QIT-TOF instrument for pseudo MS(n) strategies and top down proteomics.     

Hyperboloid mass spectrometer with a truncated trap

A hyperboloid mass spectrometer is proposed in which the analyzer is a three-dimensional ion trap truncated by the plane z=0. The mass peaks for different operating regimes of the mass analyzer are constructed from the results of a numerical modeling of the electric field and a simulation of the process of sorting the charged particles. The results serve as a basis for the construction of a hyperboloid mass spectrometer with a simple electrode system and a high resolving power. Pis’ma Zh. Tekh. Fiz. 25, 51–56 (May 26, 1999)