Mass spectroscopy detectors

Another method included in this chapter is ICP-MS, which, although not based on atomic spectroscopy in a true sense, utilizes the same instrumental approach as ICP-AES for sample introduction. The difference is that analyte quantification takes place using a mass spectroscopy detector. 

Mass and MS spectrum TGA-MS In TGA-MS, the TG is connected online with a mass spectroscopy detector to determine the nature and amount of volatile product emitted by the sample during a thermogravimetric experiment... 

Historically, measurements have classified ambient hydrocarbons in two classes methane (CH4) and all other nonmethane volatile organic compounds (NMVOCs). Analyzing hydrocarbons in the atmosphere involves a three-step process collection, separation, and quantification. Collection involves obtaining an aliquot of air, e.g., with an evacuated canister. The principal separation process is gas chromatography (GC), and the principal quantification technique is wdth a calibrated flame ionization detector (FID). Mass spectroscopy (MS) is used along with GC to identify individual hydrocarbon compounds. 

A number of analytical techniques such as FTIR spectroscopy,65-66 13C NMR,67,68 solid-state 13 C NMR,69 GPC or size exclusion chromatography (SEC),67-72 HPLC,73 mass spectrometric analysis,74 differential scanning calorimetry (DSC),67 75 76 and dynamic mechanical analysis (DMA)77 78 have been utilized to characterize resole syntheses and crosslinking reactions. Packed-column supercritical fluid chromatography with a negative-ion atmospheric pressure chemical ionization mass spectrometric detector has also been used to separate and characterize resoles resins.79 This section provides some examples of how these techniques are used in practical applications. 

The structure of the second edition follows that of the first edition, with novel applications contained in sections attached to the individual chapters. The present chapter covers mass spectroscopy, with additional applications being found in the individual chapters, as well as advances in common detectors, unusual modes of chromatography, and general theoretical advances. 

Perhaps the most revolutionary development has been the application of on-line mass spectroscopic detection for compositional analysis. Polymer composition can be inferred from column retention time or from viscometric and other indirect detection methods, but mass spectroscopy has reduced much of the ambiguity associated with that process. Quantitation of end groups and of co-polymer composition can now be accomplished directly through mass spectroscopy. Mass spectroscopy is particularly well suited as an on-line GPC technique, since common GPC solvents interfere with other on-line detectors, including UV-VIS absorbance, nuclear magnetic resonance and infrared spectroscopic detectors. By contrast, common GPC solvents are readily adaptable to mass spectroscopic interfaces. No detection technique offers a combination of universality of analyte detection, specificity of information, and ease of use comparable to that of mass spectroscopy. 

Fig. 1.3. Experimental setup for electrochemical thermal desorption mass spectroscopy (ECTDMS). C = electrochemical cell, W = working electrode, El = electrolyte inlet, EO = electrolyte outlet, EH = electrode holder, V = valve, TP = turbo pump, VC = vacuum chamber, L = light source, W = window, P = protective jacket, A = aperture to analysis chamber, GI = grid ion source, S = SEM detector.

Carbon dioxide chemisorptions were carried out on a pulse-flow microreactor system with on-line gas chromatography using a thermal conductivity detector. The catalyst (0.4 g) was heated in flowing helium (40 cm3min ) to 723 K at 10 Kmin"1. The samples were held at this temperature for 2 hours before being cooled to room temperature and maintained in a helium flow. Pulses of gas (—1.53 x 10"5 moles) were introduced to the carrier gas from the sample loop. After passage through the catalyst bed the total contents of the pulse were analysed by GC and mass spectroscopy (ESS MS). 

In mass spectroscopy, sample molecules are ionized and the different masses of the ions formed are selected by use of an electric or magnetic field. In its simplest form, a mass spectrometer is an instrument that measures the mass-to-electric charge ratios of ions formed when a sample is ionized. If some of the sample molecules are singly ionized and reach the ion detector without fragmenting, then the mass-to-electric charge ratio of the ions gives a direct measurement of the weight of the molecule (de Hoffmann and Stroobant 2001). 

Acrylonitrile in both biological and environmental samples is most commonly determined by gas chromatography with a nitrogen-phosphorus detector (GC/NPD) (Page 1985), gas chromatography/flame ionization detection (GC/FID) (EPA 1982a), or gas chromatography/mass spectroscopy (GC/MS) (Anderson and Harland 1980). Infrared spectroscopy (Jacobs and Syrjala... 

Chemicals used in this study were obtained from Aldrich Chemical Company. 1H NMR spectra were obtained on a Varian EM-360, 13C NMR spectra were obtained on a JEOL-FX-60Q or a GE QE-300. An Analect FX-6200 FT-IR spectrometer was used for infrared spectroscopy and a Hewlett-Packard Model 5980 with a model 5970 mass-selective detector was used for GC-MS. TGA measurements were performed on a Perkin-Elmer TGA-7 instrument. HPLC measurements were obtained using a Waters Instrument. 

After optimization of the correct capillary parameters (ID, OD, Lj), detection at the microscale level became the next major challenge for the survival of CE. Despite the challenges, many of the common HPLC detectors have a CE complement, e.g., absorbance, fluorescence, conductivity, photodiode array, and mass spectroscopy. Small dimensions mean universal detectors such as refractive index cannot be used. A sample of detectors will be discussed. The technical aspects of each detector will not be covered except in relation to the CE instrument. Readers are advised to consult an instrumentation textbook for more details on theory of operation. 

MS = mass spectroscopy PID = photoionization detector ppbv = parts per billion by volume... 

With today s advanced analytical procedures, it is possible to describe the composition of these fuels in considerable detail. By combining several sequenced liquid chromatographic separations with gas chromatography-mass spectroscopy and by using specific gas chromatographic detectors for sulfur compounds, it has been possible to identify the majority of individual sulfur species in some fuels (12-19). A typical separation scheme is shown... 

Recently, the word nano has become a trend in science and technology and some of us think that it is the new generation but, as mentioned above, its root is about 22 years old. NLC and NCE are gaining importance day by day. They are very useful and effective tools for samples of low quantities or having low concentrations of the analytes. Columns of low internal diameter are ideal for use in NLC and NCE, especially with detectors requiring very low flow rates, such as electrospray liquid chromatography/mass spectroscopy (LC/MS). Besides, these columns offer high sensitivity due to their low... 

AMS = accelerated mass spectroscopy FAAS = flame atomic absorption spectrometry GC/ED = gas chromatography/electron capture detector GFAAS graphite furnace atomic absorption spectrometry ICP-AES = inductively couples plasma-atomic absorption spectrometry NA = not applicable NAA = neutron activation analysis... 

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