Ion evaporation mass spectrometry

Secondary ion mass spectrometry (SIMS) has also found application in the analysis of organic compounds not prone to thermal evaporation. By this technique sulfanilic acid gave fair abundancies of [M —H] ions15, when bombarded with low primary-ion current densities on a silver target. Sulfonic acids were successfully tested by atmospheric-pressure ion evaporation mass spectrometry and found to produce characteristic negative cluster ions16. 

Thomson BA, Iribarne JV, Dziedzic PJ. Liquid ion evaporation/mass spectrometry/mass spectrometry for the detection of polar and labile molecules. Anal Chem. 1982 54 2219-24. Iribarne JV, Dziedzic PJ, Thomson BA. Atmospheric pressure ion evaporation-mass spectrometry. Int J Mass Spectrom Ion Phys. 1983 50 331-47. 

SFE-GC-MS is particularly useful for (semi)volatile analysis of thermo-labile compounds, which degrade at the higher temperatures used for HS-GC-MS. Vreuls et al. [303] have reported in-vial liquid-liquid extraction with subsequent large-volume on-column injection into GC-MS for the determination of organics in water samples. Automated in-vial LLE-GC-MS requires no sample preparation steps such as filtration or solvent evaporation. On-line SPE-GC-MS has been reported [304], Smart et al. [305] used thermal extraction-gas chromatography-ion trap mass spectrometry (TE-GC-MS) for direct analysis of TLC spots. Scraped-off material was gradually heated, and the analytes were thermally extracted. This thermal desorption method is milder than laser desorption, and allows analysis without extensive decomposition. 

Keywords Aerodynamic effects Charged droplets Cone jet Droplet evaporation Droplet deformation Electrohydrodynamic spray Electrospray Ion source Mass spectrometry Mass spectroscopy Rayleigh charge limit Spray modes Taylor cone... 

Detection methods HPLC-DAD, HPLC with diode-array detection. HPLC-(ESI-MS), HPLC with electrospray ionization mass spectrometry. RP-HPLC, revcrsed-phase HPLC. UPLC/Q-TOFMS, UPLC with quadrupole-time of flight mass spectrometry. HPLC-APCI-MS, HPLC with atmospheric pressure chemical ionization mass spectrometry. CE-IT-MS, capillary elecliophoresis-ion-1r mass spectrometry. LC-ESI-ITMS, liquid chromatography-electrospray ionization ion trap mass spectrometry. LC-ELSD, LC with evaporative light scattering detector. DNBZ-Cl, 3,5-dinitrobenzoyl chloride. 

The sample is placed on the central axis of the chamber and is accessible to LEED, AES, ESCA, ion bombardment, mass spectrometry, deposition by evaporation, and beta-radiation detection facilities. Moreover, the. sample can be rotated through 360°, thus allowing both front and back faces to be cleaned and inspected with the various surface science techniques. 

C. J. Hogan Jr. and J. FemSndez de la Mora, Tandem ion mobility-mass spectrometry (IMS-MS) smdy of ion evaporation from ionic hquid-acetonitrile nanodrops, Phys. Chem. Chem. Phys., 2009, 11, 8079-8090, 2009. 

Aerosols can be produced as a spray of droplets by various means. A good example of a nebulizer is the common household hair spray, which produces fine droplets of a solution of hair lacquer by using a gas to blow the lacquer solution through a fine nozzle so that it emerges as a spray of small droplets. In use, the droplets strike the hair and settle, and the solvent evaporates to leave behind the nonvolatile lacquer. For mass spectrometry, a spray of a solution of analyte can be produced similarly or by a wide variety of other methods, many of which are discussed here. Chapters 8 ( Electrospray Ionization ) and 11 ( Thermospray and Plasmaspray Interfaces ) also contain details of droplet evaporation and formation of ions that are relevant to the discussion in this chapter. Aerosols are also produced by laser ablation for more information on this topic, see Chapters 17 and 18. 

Dichlorodibenzo- -dioxin. 2-Bromo-4-chlorophenol (31 grams, 0.15 mole) and solid potassium hydroxide (8.4 grams, 0.13 mole) were dissolved in methanol and evaporated to dryness under reduced pressure. The residue was mixed with 50 ml of bEEE, 0.5 ml of ethylene diacetate, and 200 mg of copper catalyst. The turbid mixture was stirred and heated at 200°C for 15 hours. Cooling produced a thick slurry which was transferred into the 500-ml reservoir of a liquid chromatographic column (1.5 X 25 cm) packed with acetate ion exchange resin (Bio-Rad, AG1-X2, 200-400 mesh). The product was eluted from the column with 3 liters of chloroform. After evaporation, the residue was heated at 170°C/2 mm for 14 hours in a 300-cc Nestor-Faust sublimer. The identity of the sublimed product (14 grams, 74% yield) was confirmed by mass spectrometry and x-ray diffraction. Product purity was estimated at 99- -% by GLC (electron capture detector). 

Direct insertion probe pyrolysis mass spectrometry (DPMS) utilises a device for introducing a single sample of a solid or liquid, usually contained in a quartz or other non-reactive sample holder, into a mass spectrometer ion source. A direct insertion probe consists of a shaft having a sample holder at one end [70] the probe is inserted through a vacuum lock to place the sample holder near to the ion source of the mass spectrometer. The sample is vaporized by heat from the ion source or by heat from a separate heater that surrounds the sample holder. Sample molecules are evaporated into the ion source where they are then ionized as gas-phase molecules. In a recent study, Uyar et al. [74] used such a device for studying the thermal stability of coalesced polymers of polycarbonate, PMMA and polylvinyl acetate) (PVAc) [75] and their binary and ternary blends [74] obtained from their preparation as inclusion compounds in cyclodextrins. 

The above-mentioned method is effective in identifying the molecules of detected ions. However, because PVDF film is not permeable to light, it is difficult to observe tissue sections. To resolve this problem, we developed a method to fix tissue sections on transparent film, and then performed MS on those sections.6 We used a conductive film because we expected the ionization efficiency would increase when the electric charge accumulation on the sample was reduced. The film used for this purpose was a polyethylene terephthalate (PET) film with a thickness of 75-125 pm, having a 5 15-nm-thick layer of evaporated oxidation indium tin (ITO) upon it (ITO film). This film is used in touch-panel displays because of its high transparency and superior conductivity. We used it to perform MS/MS for tissue sections and succeeded in identifying multiple proteins from mass spectra.6 Therefore, the further development of this method will enable the application of the mass-microscopic method to observe tissue by optical microscope and to perform tandem mass spectrometry (MSn) at the observation part, simultaneously, enabling the identification of molecules included the part. 

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