Nebulization gas

HR-ICP-MS EEEMENT-2 (Pinnigan MAT, Germany) equipped with a standard introduction system (quartz water-cooled spray chamber, concentric nebulizer, torch with 1.5 mm i.d. injector and nickel cones) was used for measurements. The following operating conditions were used RP power 1150 W, coolant gas flow rate 16 1 min k auxiliary gas flow rate 0.85 1 min nebulizer gas flow rate 1.2 1 min k Sample uptake rate was 0.8-1 ml min k Measurements were performed with low and middle resolutions. Rh was used as an internal standard. Por calibration working standard solutions were prepared by diluting the multielemental stock solutions CPMS (SPEX, USA) with water to concentration range from 5 ng to 5 p.g I k... 

The most important feature of any interface which is capable of allowing an El spectrum to be produced is that the mobile phase is totally removed so that the spectra obtained may be attributed solely to the analyte. Whether or not this is accomplished depends upon the composition of the mobile phase, its flow rate and the conditions employed within the interface, i.e. temperature, nebulizing gas flow, etc. 

A thermospray system is shown schematically in Figure 4.6. This consists of a heated capillary through which the LC eluate flows, with the temperature of this capillary being carefully controlled to bring about around 95% vaporization of the liquid. The vapour so produced acts as a nebulizing gas and aids the break-up of the liquid stream into droplets. 

Atmospheric-pressure chemical ionization (APCI) is another of the techniques in which the stream of liquid emerging from an HPLC column is dispersed into small droplets, in this case by the combination of heat and a nebulizing gas, as shown in Figure 4.21. As such, APCI shares many common features with ESI and thermospray which have been discussed previously. The differences between the techniques are the methods used for droplet generation and the mechanism of subsequent ion formation. These differences affect the analytical capabilities, in particular the range of polarity of analyte which may be ionized and the liquid flow rates that may be accommodated. 

Factors may be classified as quantitative when they take particular values, e.g. concentration or temperature, or qualitative when their presence or absence is of interest. As mentioned previously, for an LC-MS experiment the factors could include the composition of the mobile phase employed, its pH and flow rate [3], the nature and concentration of any mobile-phase additive, e.g. buffer or ion-pair reagent, the make-up of the solution in which the sample is injected [4], the ionization technique, spray voltage for electrospray, nebulizer temperature for APCI, nebulizing gas pressure, mass spectrometer source temperature, cone voltage in the mass spectrometer source, and the nature and pressure of gas in the collision cell if MS-MS is employed. For quantification, the assessment of results is likely to be on the basis of the selectivity and sensitivity of the analysis, i.e. the chromatographic separation and the maximum production of molecular species or product ions if MS-MS is employed. 

In APCI, droplets are generated by a combination of heat and a nebulizing gas. While the analytes are embedded in a droplet, and thus protected to some extent from the heat, many thermally labile materials are decomposed. In addition, ionization occurs mainly by ion-molecule reactions and yields predominantly singly charged ions. If, therefore, compounds do not undergo thermal degradation, a mass spectrometer with extended mass range would be required to detect any ions formed. 

Aerospray An atmospheric-pressure ionization technique in which droplets are formed from a liquid stream by a combination of heat and a nebulizing gas and ions are formed by ion evaporation ramer man ion-molecule reactions. 

Atmospheric-pressure chemical ionization (APCI) An ionization memod in which a liquid stream is passed through a heated capillary and a concentric flow of a nebulizing gas. Ions are formed by ion-molecule reactions between me analyte and species derived from me HPLC mobile phase. 

Flow rate Injection volume Retention time Ionization mode Polarity Nebulizer gas Auxiliary gas Nebulizer temperature Collision gas Acquisition... 

The multiple reaction monitoring (MRM) conditions for each analyte were optimized by infusing 0.1 jxglmL of analyte in mobile phase. The Ionspray needle was maintained at 4.0 kV and the turbo gas temperature was 650°C. Nebulizing gas, auxiliary gas, curtain gas, and collision gas flows were set at 35, 35,40, and 4, respectively. In the MRM mode, collision energies of 17,16, and 15 eV... 

Figure 4.8 Schematic of an electrospray probe with a concentric flow of nebulizing gas. From applications literature published by Micromass UK Ltd, Manchester, UK, and reproduced with permission.

Ionspray Pneumatically assisted electrospray - a process in which nebulizing gas is used in conjunction with a high voltage to form droplets from a liquid stream. 

The significant enhancement of ion formation by a corona discharge as compared to a Ni source has already been implemented in early API sources. [139,140] The nature of the APCI plasma varies widely as both solvent and nebulizing gas contribute to the composition of the Cl plasma, i.e., APCI spectra can resemble PICI, CECI, NICI, or EC spectra (Chap. 7.2-7.4) depending on the actual conditions and ion polarity. This explains why APCI conditions suffer from comparatively low reproducibility as compared to other ionization methods. 

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