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1.
Anal Chem ; 87(6): 3115-22, 2015 Mar 17.
Artigo em Inglês | MEDLINE | ID: mdl-25708099

RESUMO

Miniaturized mass spectrometers are becoming increasingly capable, enabling the development of many novel field and laboratory applications. However, to date, triple quadrupole tandem mass spectrometers, the workhorses of quantitative analysis, have not been significantly reduced in size. Here, the basis of a field-deployable triple quadrupole is described. The key development is a highly miniaturized ion optical assembly in which a sequence of six microengineered components is employed to generate ions at atmospheric pressure, provide a vacuum interface, effect ion guiding, and perform fragmentation and mass analysis. Despite its small dimensions, the collision cell efficiently fragments precursor ions and yields product ion spectra that are very similar to those recorded using conventional instruments. The miniature triple quadrupole has been used to detect thiabendazole, a common pesticide, in apples at a level of 10 ng/g.

2.
Rapid Commun Mass Spectrom ; 25(21): 3281-8, 2011 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-22006391

RESUMO

A miniature mass spectrometer capable of detecting analytes eluting from a high-performance liquid chromatography (HPLC) system is described and demonstrated for the first time. The entire instrument, including all pumps and the computer, is contained within a single enclosure that may be conveniently accommodated at the base of the HPLC stack. The microspray ion source, vacuum interface, ion guide, and quadrupole ion filter are all microengineered. These components are fabricated in batches using microelectromechanical systems (MEMS) techniques and considered to be consumables. When coupled to a standard HPLC system using an integrated passive split, the limit of detection for reserpine while scanning the full mass range is 5 ng on-column (1 pg of which is passed to the microspray). The mass range is m/z 100-800, and each spectrum is typically acquired at a rate of 1 scan per second.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas/instrumentação , Sistemas Microeletromecânicos/instrumentação , Miniaturização/instrumentação , Espectrometria de Massas/métodos , Modelos Químicos , Reserpina/análise , Sensibilidade e Especificidade
3.
Anal Chem ; 82(5): 1751-8, 2010 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-20108919

RESUMO

Two miniature mass spectrometer systems based on a microengineered quadrupole mass filter have been developed. One of the instruments has a footprint of 27 cm x 20 cm and is intended for laboratory use when space is at a premium. The other is portable and intended for use in the field. It is battery powered, weighs 14.9 kg, and is housed in a rugged case. This is the first example of a portable mass spectrometer incorporating an analyzer fabricated using microelectromechanical systems (MEMS) techniques. The starting material for construction of the filters is a bonded silicon on insulator substrate, which is selectively etched using batch processing techniques to form coupling optics and springs that accurately hold 0.5 mm diameter stainless steel rods in the required geometry. Assembled filters measure 35 mm x 6 mm x 1.5 mm and are mounted, together with an ion source and channeltron detector, in small, interchangeable cartridges, which plug into a 220 cm(3) vacuum chamber. Recovery from accidental contamination or when servicing is required can be achieved within 5-10 min, as the cartridge is easily exchanged with a spare. A potential application to environmental monitoring has been investigated. The headspace above water spiked with dibutyl mercaptan was sampled with a solid phase microextraction (SPME) fiber, which was then injected directly into the vacuum chamber of the mass spectrometer. Using this method, the limit of detection was found to be approximately 5 ppm for a 15 s sampling period.

4.
Phys Rev E Stat Nonlin Soft Matter Phys ; 68(1 Pt 2): 016408, 2003 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-12935259

RESUMO

Ions created from the fast-flowing positive column plasma of a glow discharge were monitored using a high voltage magnetic sector mass spectrometer. Since the field gradient and sheath potentials created by the plasma inside the source opposed cation transfer, it is inferred that the ions detected were the field-ionized Rydberg species. This is supported by the mass spectral changes which occurred when a negative bias was applied to the sampling aperture and by the contrasting behavior when attached to a quadrupole analyzer. Reaction with H2 (titrated into the flowing plasma) quenched not only the ionization of discharge gas Rydberg atoms but also the passage of electric current through the plasma, without significant changes to the field and sheath potentials. Few "free" ions were present and the lifetimes of the Rydberg atoms detected were much longer than seen in lower pressure experiments, indicating additional stabilization in the plasma environment. The observations support the model of the flowing plasma, given previously [R. S. Mason, P. D. Miller, and I. P. Mortimer, Phys. Rev. E 55, 7462 (1997)] as mainly a neutral Rydberg atom gas, rather than a conventional ion-electron plasma.

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