Survey scan

Figure 2. Negative FAB mass spectra of maitotoxin. The numbers denote the mass number at the centroid of each peak. A A survey scan at a low resolution (R=300). B. Resolution enhanced spectrum (R=3000) for ion clusters at around m/z 3300. C. Resolution enhanced spectrum (R=3000) for ion clusters at around miz 3400.

Whilst qualitative survey scans are useful in the preliminary analytical investigations of a problem, the extent to which such signals can be quantified is of greater importance. Unless the sample matrix is simple,... 

The mounted samples were placed in the XPS vacuum chamber, and the chamber was evacuated prior to testing. The samples were exposed to the X-rays at 14.0 kV and 300 W. The approximate sampling area for the XPS is 1.0mmx3.5mm with a sampling depth of approximately 35.0 A at a 45° exit angle. Figures 16 and 17 show the survey scans from the epoxy and composite sample, respectively. Both show the presence of fluorine, which indicates the probable presence of a mold-release agent. 

Data-dependent acquisition ability has been developed and incorporated into most software packages [MetaboLynx, Xcalibur, and Analyst Information Dependent Acquisition (IDA)]. In data-dependent acquisition mode, a mass spectrometer decides on the fly whether to collect MS/MS or MSn data, remain in full scan MS mode, or conduct other survey scans based upon user-defined criteria. Product ion spectra of potential metabolites can be automatically acquired in a single LC/ MS run. However, false positives may be generated due to highly intense matrix ion signals that may inadvertently trigger MS/MS or MSn scan functions. 

Figure 1, for example, shows a survey scan of natural galena,... 

Figure 1. X-ray photoelectron survey scan of naturally weathered galena, PbS.

The major advantage of this instrument is that qualitative and quantitative analysis can be performed in the same LC-MS run. As an example in a data-dependent experiment, the selected reaction monitoring mode can be used as a survey scan and the enhanced product ion mode (EPI) as a dependent scan. The consequence is that for each quantified analyte a confirmatory MS/MS spectmm can be obtained. 

In this case the survey scan was set as a full scan and the dependent scan as a product ion scan. The problem with data dependent acquisition is to determine the selection criteria. In most cases the system picks up the most abundant ion in the full scan spectrum. An inclusion list with masses of potential metabolites or exclusion list of known interferences significantly improves the procedure. In the example shown in Fig. 1.39, a procedure called dynamic background subtraction (DBS) was applied. This procedure considers chromatographic peak shapes and monitors not the most abundant signal in the spectrum but the largest increase of an ion in a spectrum. The advantage is that once a signal of a peak has... 

Fig. 1.39 LC-MS data dependent analysis of vinpocetin in rat urine using dynamic background substraction (DBS) on a triple quadrupole linear ion trap. (A) Full scan MS (survey scan) trace. (B) Enhanced product ion scan (dependent scan). The major peak at 3.9 min corresponds to apovinpocetin, the minor one at 2.9 min to the hydroxylation product of apovinpocetin (m/z 339).

The XPS data were obtained with an extensively modified AEI ES-100 photoelectron spectrometer. The samples were analyzed at a pressure typically < 10 g Torr. A magnesium anode (1253.6 eV) was used as the excitation source. The analyzed sample area was of the order of 5 mm2. Survey scans from 0 to 1000 eV were first obtained for each sample to confirm that only the expected elements were present on the fiber surfaces. Subsequently, high resolution spectra were obtained by slowly scanning — 20 eV binding energy windows that included the Si 2p, Al 2p, Ca 2p, B Is, O Is, and C Is photoelectrons, respectively. Integrated peak areas of the photoelectron spectra were determined. The sensitivity factors, which were independently obtained on this spectrometer with oxide standards, were then utilized in the determination of the surface atomic percent compositions of the fibers. 

ESCA survey scans recorded for thermal oxide surfaces indicated the presence of Si, C, and O. The elemental compositions for these oxides are similar to those for the Y58 blank system of Table 5. Again, the simple elemental compositions do not show any dramatic changes due to the surface chemical modifications by... 

A new generation of linear ion trap mass spectrometers has been developed and exhibits increased performance compared to traditional three-dimensional (3D) ion traps (Hopfgartner et al., 2003 Douglas et al., 2005). A further evolution of the triple-quadrupole family and ion trap class of instruments is the production of the hybrid triple-quadrupole/linear ion trap (QQQ/LIT) platform. Hybrid instruments of this nature allow for operation in space and not just in time when performing MS/MS analysis. This feature allows for increased performance compared to classical ion traps. A powerful combination possible on a hybrid LIT/QQQ instrument is the ability to use highly sensitive and selective precursor ion, constant neutral loss, and multi-MRM as a survey scan for dependent LIT MS/MS. Compared to a simple MS experiment, these comprehensive triple-quadrupole and LIT modes can be more complex to setup. 

Figure 3.19. Comparison of S/N for glucuronide metabolite of testosterone detected using different IDA survey scans.

An example of such an analysis of rhodium phosphine ligand anchored catalysts is presented (58). A survey scan of a copolymer containing a diphosphine ligand prior to introduction of the metal is shown in Figure 1, spectrum h. The presence of phosphorus in the polymer is evident from this spectrum. 

Figure 9.15. Influence of sample cleaning on XPS scans taken on a thin-film superconductor, (a) Survey scan from an as-received surface, (b) Survey scan from surface after ion-beam (sputter) cleaning. Note the reduction in the Cls peak after cleaning, (c) Comparative Ba3d scans from both cases. Note the change in shape and size as the surface contaminant layers (probably containing carbonates and hydroxides of Ba in addition to other components) are removed. The peak shapes and intensities of other cations change, too. Initial data represent the composition and chemistry of the contaminant layer, whereas that from sputtered sample represents those of the pure underlying superconductor (possibly with sputter-induced changes that need to be accounted for).

FIGURE 21 ESCA spectrum of a palladium-on-carbon catalyst. A, Survey scan locating the carbon 1s and the palladium 3pand 3d peaks B, scale expansion around the palladium 3d doublet. The small shoulder at the oxide location is assigned to a chemisorbed oxygen state. 

Fig. 8. The XPS survey scan spectra of the changes in the surface chemical compositions through the micropatterning process.

The scattering cylinder of the focused laser beam must be aligned vertically to be parallel to the entrance slit of the spectrometer. The collection lens is used to image this cylinder onto the slit. The sample is then inserted at the laser focal point with its long axis parallel to the beam and a quick survey scan is taken until a Raman band is found. The sample, the excitation beam, and the collection lens are then carefully adjusted for maximum signal at this spectrometer setting. 

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