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 train of six microengineered components are employed to generate ions at atmospheric pressure, provide a vacuum interface, effect ion guiding, and perform pre-filtering, 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 instrument has been used to detect Thiabendazole, a common pesticide, in apple pulp at a level of 10 ppb.3

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.

An electrospray ionisation mass spectrometer (ESI-MS) whose main components are all fabricated using silicon microelectromechanical systems (MEMS) techniques is demonstrated for the first time. The ion source consists of a microengineered alignment bench containing a V-groove mounting for a nanospray capillary, an ion extraction electrode, and a pneumatic nebuliser. The vacuum interface consists of two plates, each carrying a 50 µm diameter capillary, that are selectively etched and bonded together to provide a differentially pumped internal cavity. The quadrupole filter consists of a microfabricated frame that provides mountings for stainless steel rods measuring 650 µm in diameter and 30 mm in length. Two different quadrupoles are compared: a firstgeneration bonded silicon device, and a second-generation silicon-on-glass device with a Brubaker prefilter. Differential pumping of a MEMS component is demonstrated for the first time, atmospheric pressure ionisation and ion transfer into vacuum are characterised, ESI-MS operation is demonstrated and spectra are presented for a variety of compounds. KEYWORDS:Mass spectrometry, Electrospray, Quadrupole filter, MEMS IntroductionOver 25 years have passed since an electrospray ionisation (ESI) source was first coupled to a quadrupole mass spectrometer (MS) by Yamashita and Fenn [1]. Since then, ESI-MS has become a workhorse of analytical chemistry, allowing analytes to be ionised at atmospheric pressure with little fragmentation and passed into a vacuum system for analysis.Conventional ESI sources employ spray tips with an internal diameter (ID) of ≈100 µm[2]. In order to establish a Taylor cone and maintain stable emission of charged droplets, minimum flow rates of 0.5 -5 µL min -1 and voltages of 2.5 -4 kV are used. However, it has been convincingly demonstrated that high sensitivity and stable emission can be achieved at much lower flow rates and voltages using spray tips with IDs of ≈ 5 µm, and silica nanospray capillaries with a range of coatings have become widely available [3][4][5][6][7][8].Unfortunately, while these are inexpensive, operator expertise and costly positioning apparatus are often required for stable and reproducible performance.Electrosprayed ions are passed into a low-pressure chamber via a vacuum interface. The simplest interface is a single orifice or capillary that allows gas and entrained ions to pass directly into the vacuum chamber. Clearly, the orifice must be small enough or the pumps large enough to ensure that the pressure is consistent with mass analysis. However, the susceptibility of very small orifices to clogging and the inconvenience of large pumps led to this approach being abandoned. Modern instruments employ one or more stages of 4 differential pumping. Larger orifices can be tolerated since only a fraction of the flow is transmitted to the vacuum chamber, while the majority of the gas load can be pumped away at higher pressure using more modest pumps.The effective transfer of ions and molecules from atmospheric pressu...

Using a focused ion beam, we have produced superconductor-normal metal-superconductor junctions by controllably removing a portion of the top layer of a patterned superconductor-normal metal thin film. The high-quality junctions showed Josephson coupling which scaled qualitatively with barrier properties and temperature as expected. The largest product of a junction’s critical current and the normal state resistance measured is 98 μV at 4.2 K. The method has good reproducibility and could be exploited in a number of superconducting electronics applications.

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