Mass analyzers vacuum systems

The ionic current intensity corresponding to the peak at 169 amu was analyzed under isothermal and polythermal conditions [383]. It was found that in a gaseous atmosphere, the intensity changes are in correlation with the CO content and in negative correlation with the C02 content. The presence of CO in vacuum systems equipped with heating elements is usually related to thermo-cycling and desorption of CO by nickel atoms [386]. Based on the above, the presence of NbF4+ ions in mass spectra is most probably related to the niobium reduction process, which can be represented as follows ... 

The MC-ICP-MS consists of four main parts 1) a sample introduction system that inlets the sample into the instrument as either a liquid (most common), gas, or solid (e.g., laser ablation), 2) an inductively coupled Ar plasma in which the sample is evaporated, vaporized, atomized, and ionized, 3) an ion transfer mechanism (the mass spectrometer interface) that separates the atmospheric pressure of the plasma from the vacuum of the analyzer, and 4) a mass analyzer that deals with the ion kinetic energy spread and produces a mass spectrum with flat topped peaks suitable for isotope ratio measurements. 

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. 

Fig. 1.8 Di fferential pumping design with heated capilla. This configuration requires a dual stage pumping system before the ions are introduced into the quadrupole mass analyzer which needs to be operated at high vacuum. The role of the lenses is to focus ions. In some systems the lenses are replaced by hexapoles or octapoles.

The LC column can operate for several weeks without any loss of separation efficiency. The flow rate of solvent into the mass spectrometer is 2-3 pL/min under normal conditions. The pressure in the ion source housing is 10 Pa and 10 Pa in the analyzer. No deterioration of the vacuum system during two years of operation has been observed. 

In IC-MS systems, the core of the equipment is the interface. In fact, inside the interface evaporation of the liquid, ionization of neutral species to charged species and removal of a huge amount of mobile phase to keep the vacuum conditions required from the mass analyzer take place. Two main interfaces are used coupled to IC, namely electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI). In the ESI mode, ions are produced by evaporation of charged droplets obtained through spraying and an electrical field, whilst in the APCI mode the spray created by a pneumatic nebulizer is directed towards a heated region (400°C-550°C) in which desolvation and vaporization take place. The eluent vapors are ionized by the corona effect (the partial discharge... 

The sample to be analyzed is introduced to the ESI source by means of a flow stream from an HPLC instrument. The sample flows through a stainless-steel needle and then, sprays out in the form of a mist whose droplets hold peptide ions and mobile phase of HPLC. Peptide ions are separated from the mobile phase and subsequently, transferred into a mass analyzer either by a heated capillary or a curtain of nitrogen gas. Desolvation process can be carried out by a vacuum system. 

A second important property of mass spectrometric separation systems is the abundance sensitivity. Even under sufficient vacuum conditions there is a scattering of ions in the beam by the residual gas. Furthermore, by scattering of particles by the wall of the analyzer tube or by electrostatic repulsion in the ion beam itself or charging effects, so-called peak tails in mass spectra are observed, which result in an increasing energy spread of ions and consequently in a deterioration in the abundance sensitivity. The abundance sensitivity of a mass spectrometer is defined as ... 

When the separated ion beams leave the mass analyzer system the ions are collected and detected using an appropriate ion detection system inserted in the ultrahigh vacuum of the mass spectrometer. Ion currents at the exit of the mass analyzer are in the range of 10 8 to 10 19 A. The registration of both high and very small ion currents requires special fast ion detection systems as discussed in this chapter. 

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