Quadrupole mass detector

There are many types of mass spectrometer, from high-resolution double-focusing instruments, which can distinguish molecular and fragment masses to six decimal places, to bench-top machines with a quadrupole mass detector which can resolve masses up to about m/z = 500, but only in whole-number differences. Routinely you are most likely to encounter data from bench-top instruments and therefore only this typie of spectrum will be considered. 

Quadrupole mass spectrometers (mass filters) allow ions at each m/z value to pass through sequentially for example, ions at m/z 100, 101, 102 will pass one after the other through the quadrupole assembly so that first m/z 100 is transmitted, then m/z 101, then m/z 102 (or vice versa), and so on. Therefore, the ion collector (or detector) at the end of the quadrupole unit needs to cover only one point or focus in space (Figure 29.1a), and a complete mass spectrum is recorded over a period of time. The ions arrive at the collector sequentially, and ions are detected in a time domain, not in a spatial domain. 

For IBSCA analysis, standard HV or, better, UHV-equipment with turbomolecular pump and a residual gas pressure of less than 10 Pa is necessary. As is apparent from Fig. 4.46, the optical detection system, which consists of transfer optics, a spectrometer, and a lateral-sensitive detector, is often combined with a quadrupole mass spectrometer for analysis of secondary sputtered particles (ions or post-ionized neutrals). 

Accessibility to Cu sites was determined by temperature programmed desorption of NO (NO TPD), using an experimental setup similar to that used for TPR, except the detector was a quadrupole mass spectrometer (Balzers QMS421) calibrated on standard mixtures. The samples were first activated in air at 673 K, cooled to room temperature in air, and saturated with NO (NO/He 1/99, vol/vol). They were then flushed with He until no NO could be detected in the effluent, and TPD was started up to 873 K at a heating rate of 10 K/min with an helium flow of 50 cm min. The amount of NO held on the surface was determined from the peak area of the TPD curves. 

Chromatographic systems were finally coupled with relatively inexpensive, yet powerful, detection systems with the advent of the quadrupole mass selective detector (MSD). The operational complexity of this type of instrumentation has significantly declined over the last 15 years, thus allowing routine laboratory use. These instruments... 

In the early 1970s, the introduction of the quadrupole mass spectrometer changed the landscape of residue analysis in the coming decades dramatically. The combination of GLC with the mass spectrometer as a detector proved to become the major tool for residue analysis for the next 20 years. 

Gas chromatograph fitted with a thermionic nitrogen-specific detector Gas chromatograph fitted with a quadrupole mass-selective detector... 

Fieiure 9-1 Schematic view of (A) the bench-top quadrupole mass spectrometer (Hewlett-Packard) and (B) the ion trap detector (Finnigan MAT). 

Schematic representation of the experimental setup is shown in Fig 1.1. The electrochemical system is coupled on-line to a Quadrupole Mass Spectrometer (Balzers QMS 311 or QMG 112). Volatile substances diffusing through the PTFE membrane enter into a first chamber where a pressure between 10 1 and 10 2 mbar is maintained by means of a turbomolecular pump. In this chamber most of the gases entering in the MS (mainly solvent molecules) are eliminated, a minor part enters in a second chamber where the analyzer is placed. A second turbo molecular pump evacuates this chamber promptly and the pressure can be controlled by changing the aperture between both chambers. Depending on the type of detector used (see below) pressures in the range 10 4-10 5 mbar, (for Faraday Collector, FC), or 10 7-10 9 mbar (for Secondary Electrton Multiplier, SEM) may be established.

The concept of peak capacity is rather universal in instrumental analytical chemistry. For example, one can resolve components in time as in column chromatography or space, similar to the planar separation systems however, the concept transcends chromatography. Mass spectrometry, for example, a powerful detection method, which is often the detector of choice for complex samples after separation by chromatography, is a separation system itself. Mass spectrometry can separate samples in time when the mass filter is scanned, for example, when the mass-to-charge ratio is scanned in a quadrupole detector. The sample can also be separated in time with a time-of-flight (TOF) mass detector so that the arrival time is related to the mass-to-charge ratio. 

As with all spectroscopic methods discussed previously, this method is best suited to measurement and elucidation of the characteristics of pure compounds. For this reason, MS is often used as a detector for gas chromatographs. The GC separates the mixture into pure compounds and the MS then analyzes each pure chemical as it exits the column. The most common MS for this application is the quadrupole mass spectrometer. For this reason, it is discussed in Chapters 14 and 15. 

In the past decade, as systems have become simpler to operate, mass spectrometry (MS) has become increasingly popular as a detector for GC. Of all detectors for GC, mass spectrometry, often termed mass selective detector (MSD) in bench-top systems, offers the most versatile combination of sensitivity and selectivity. The fundamentals of MS are discussed elsewhere in this text. Quadrupole (and ion trap, which is a variant of quadrupole) mass analyzers, with electron impact ionization are by far (over 95%) the most commonly used with GC. They offer the benefits of simplicity, small size, rapid scanning of the entire mass range and sensitivity that make an ideal detector for GC. 

We discussed the fundamentals of mass spectrometry in Chapter 10 and infrared spectrometry in Chapter 8. The quadrupole mass spectrometer and the Fourier transform infrared spectrometer have been adapted to and used with GC equipment as detectors with great success. Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-infrared spectrometry (GC-IR) are very powerful tools for qualitative analysis in GC because not only do they give retention time information, but, due to their inherent speed, they are also able to measure and record the mass spectrum or infrared (IR) spectrum of the individual sample components as they elute from the GC column. It is like taking a photograph of each component as it elutes. See Figure 12.14. Coupled with the computer banks of mass and IR spectra, a component s identity is an easy chore for such a detector. It seems the only real... 

Fig. 2. Schematic diagram of a high resolution He time-of-flight spectrometer. N-nozzle beam source, SI, 2-skimmers, Al-5 - apertures, T - sample, G - gas doser, CMA - Auger Spectrometer, IG - ion gun, L - LEED, C -magnetically suspended pseudorandom chopper, QMA-detector, quadrupole mass analyzer with channeltron.

Recently, comparatively inexpensive, very reliable, and stable single quadrupole mass spectrometers have entered the market. These spectrometers can be coupled to GC, LC, and CE separation methods simply by modifying the sampling interfaces. Although these detectors are more expensive than most conventional detectors including the versatile electron capture and diode array absorbance detectors used for GC and LG respectively, the reduction in sample preparation effort and their increased specificity can often rapidly... 

---