Vacuum systems sources

Direct-inlet probe. A shaft or tube having a sample holder at one end that is inserted into the vacuum system of a mass spectrometer through a vacuum lock to place the sample near to, at the entrance of, or within the ion source. The sample is vaporized by heat from the ion source, by heat applied from an external source, or by exposure to ion or atom bombardment. Direct-inlet probe, direct-introduction probe, and direct-insertion probe are synonymous terms. The use of DIP as an abbreviation for these terms is not recommended. 

Moving-belt (ribbon or wire) interface. An interface that continuously applies all, or a part of, the effluent from a liquid chromatograph to a belt (ribbon or wire) that passes through two or more orifices, with differential pumping into the mass spectrometer s vacuum system. Heat is applied to remove the solvent and to evaporate the solute into the ion source. 

Titanium hydride is used as a source for Ti powder, alloys, and coatings as a getter in vacuum systems and electronic tubes as a sealer of metals and as a hydrogen source. 

Ultrasound frequencies can be introduced into the walls of the vacuum system. If a source of ultrasound is placed on the wall of an ultrahigh vacuum system, a large hydrogen peak is observed. Related phenomena, presumably from frictional effects, are observed if the side of a vacuum system is tapped with a hammer a desorption peak can be seen. Mechanical scraping of one part on another also produces desorption. 

Vacuum systems, largely for the semiconductor industry, are the main source of sales (see Semiconductors). The sales of all vacuum equipment, pumps (qv), valves, sensors (qv), etc, in the United States, including apphcations not in vacuum systems, generally exceed 500 X 10 /yr. A reasonably comprehensive hst of high vacuum manufacturers is supphed by the American Vacuum Society s exhibitor s hst. In Europe, a special issue of the journal A acuum serves similady. 

Vacuum systems (Fig. 21-12h) are characterized by material moving in an air stream of pressure less than ambient. The advantages of this type are that all the pumping energy is used to move the product and that material can be sucked into the conveyor line without the need of a rotaiy feeder or similar seal between the storage vessel and the conveyor. Material remains suspended in the air stream until it reaches a receiver. Here, a cyclone separator or filter (Fig. 21-12c) separates the material from the air, the air passing through the separator and into the suction side of the positive-displacement blower or some other power source. 

Vacuum systems are typically used when flows do not exceed 6800 kg/h (15,000 Ib/h), the equivalent conveyor length is less than 305 m (1000 ft), and several points are to be supplied from one source. They are widely used for finely divided materi s. Of special interest are vacuum systems designed for flows under 7.6 kg/min (1000 Ib/h), used to transfer materials short distances from storage bins or bulk containers to process units. This type of conveyor is widely used in plastics and other processing operations where the variety of conditions requires flexibility in choosing pickup devices, power sources, and receivers. Capital investment can be kept low, often in the range of 2000 to 7000. 

Different options are available for LC-MS instruments. The vacuum system of a mass spectrometer typically will accept liquid flows in the range of 10-20 p,L min-1. For higher flow-rates it is necessary to modify the vacuum system (TSP interface), to remove the solvent before entry into the ion source (MB interface) or to split the effluent of the column (DLI interface). In the latter case only a small fraction (10-20 iLrnin ) of the total effluent is introduced into the ion source, where the mobile phase provides for chemical ionisation of the sample. The currently available commercial LC-MS systems (Table 7.48) differ widely in characteristics mass spectrometer (QMS, QQQ, QITMS, ToF-MS, B, B-QITMS, QToF-MS), mass range m/z 25000), resolution (up to 5000), mass accuracy (at best <5ppm), scan speed (up to 13000Das-1), interface (usually ESP/ISP and APCI, nanospray, PB, CF-FAB). There is no single LC-MS interface and ionisation mode that is readily suitable for all compounds... 

Figure 4-4 shows a typical system under positive pressure. It differs from the vacuum system in that the material enters from one source and is distributed directly to several tanks. In this case no cyclone separator is used the air laden with solids enters the process bins directly. The decrease in velocity of the stream and its change in direction will cause most of the solids to drop out. For this system each receiver must have a filter to remove the remaining solids. Note that the blower is placed at the air entrance, instead of after the filter as in the vacuum system. Should a bag in the fiber filter break, no dust will get into the blower or its motor. Another advantage is that no contaminants from the atmosphere can enter the system when it is under positive pressure, except through the air inlet system. 

Fig. 1. Schematics of an electrospray ion trap mass spectrometer. The ions produced from the electrospray ion source are transferred into the vacuum system of the mass spectrometer and guided into the trapping region where they are stored. After storage they can be scanned toward the detector to generate a mass spectrum. Alternatively, ions of a single m/z can be stored inside the trap, accelerated so that they fragment on collision with restgas molecules, and the fragments can be scanned toward the detector to determine their mass.

Example The vacuum system of non-benchtop mass spectrometers consists of one to three rotary vane pumps and two or three turbo pumps. Rotary vane pumps are used for the inlet system(s) and as backing pumps for the turbo pumps. One turbo pump is mounted to the ion source housing, another one or two are operated at the analyzer. Thereby, a differentially pumped system is provided where local changes in pressure, e.g., from reagent gas in Cl or collision gas in CID, do not have a noteworthy effect on the whole vacuum chamber. 

In early GC-MS with paeked GC columns eluting several tens of milliliters per minute most of the flow had to be separated before entering the ion source to prevent the vacuum system from breakdown. [4,29,34] This was either effected by a simple split to divide the effluent in front of the inlet system by a faetor of about 1 100 or by means of a more elaborate separator, the jet separator being the best... 

There are five major components of a mass spectrometer coupled to a GC. They are, vacuum system, ion source, mass filter, detector, and data system. 

The DLI interface became the second commercially available LC/MS interface in 1981. The liquid eluent is introduced into the ion source through a capillary or a pinhole diaphragm. As the name implies, the analyte in DLI LC/MS is introduced from solution into the MS ion source.When sufficient energy is given to the solution, the preformed ions in solution such as protonated molecules, deprotonated molecules, cationized molecules and solvated ions can be desorbed into a mass spectrometer while the bulk solvent is vaporized and eliminated by the vacuum system. 

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