Inductively coupled plasma/selected ion

Catalytic activity in the homogeneous gas-phase conversion of nitrogen oxides and carbon monoxide to nitrogen and carbon dioxide was observed to be most effective for the atomic ions Fe+, Os+, and Ir+ out of the investigation of 29 different transition metal cations M+ [462]. The overall catalytic scheme that was established in this study consists of the three catalytic cycles shown in Fig. 1.94. The catalysis occurs in two steps in which NO is first reduced to N2O. An analogous three-step catalytic reduction of NO2, in which NO2 is first reduced to NO, was also discovered. The three cycles in Fig. 1.94 were characterized with laboratory measurements of reactions of each of the three nitrogen oxides NO2, NO, and N2O with the different transition metal ions in an inductively coupled plasma/selected-ion flow tube tandem mass spectrometer [462]. 

ICP/SIFT inductively coupled plasma/selected-ion flow tube... 

Koyanagi, G.K., Lavrov, VV, Baranov, V. et al. (2000) A novel inductively coupled plasma/selected-ion flow tube mass spectrometer for the study of reactions of atomic and atomic oxide ions. Int. J. Mass Spectrom., 194, LI—L5. 

Koyanagi, G. K., Baranov,V. I., Tanna S. D., and Bohme, D. K. (2000) An inductively coupled plasma/selected-ion flow tube mass spectrometric study of the chemical resolution of isobaric interferences. J. Anal. At. Spectmm., 15,1207. 

Oxygen and nitrogen also are deterrnined by conductivity or chromatographic techniques following a hot vacuum extraction or inert-gas fusion of hafnium with a noble metal (25,26). Nitrogen also may be deterrnined by the Kjeldahl technique (19). Phosphoms is determined by phosphine evolution and flame-emission detection. Chloride is determined indirecdy by atomic absorption or x-ray spectroscopy, or at higher levels by a selective-ion electrode. Fluoride can be determined similarly (27,28). Uranium and U-235 have been determined by inductively coupled plasma mass spectroscopy (29). 

A novel interface to connect a ce system with an inductively coupled plasma mass spectrometric (icpms) detector has been developed (88). The interface was built using a direct injection nebulizer (din) system. The ce/din/icpms system was evaluated using samples containing selected alkah, alkaline earths, and heavy-metal ions, as well as selenium (Se(IV) and Se(VI)), and various inorganic and organic arsenic species. The preliminary results show that the system can be used to determine metal species at ppt to ppb level. 

L. S. Milstein, A. Essader, E. D. Pellizzari, R. A. Fernando, and O. Akinbo. Selection of a Suitable Mobile Phase for the Speciation of Four Arsenic Compounds in Drinking Water Samples Using Ion-exchange Chromatography Coupled to Inductively Coupled Plasma Mass Sectrometry. Environ, lnt., 28(2002) 277-283. 

Sample preparation for analysis by hyphenated methods requires some additional planning when compared to nonhyphenated methods. All steps, extraction, concentration, and final solvent selection must take into consideration and be compatible with all the components of the hyphenated instrumentation. For gas chromatographic methods, all the components in the mixture must be in the gaseous state. For liquid chromatography (LC) or high-performance liquid chromatography (HPLC), the samples of the analytes of interest can be solids or liquids, neutral or charged molecules, or ions, but they must be in solution. If the follow-on analysis is by MS, then each of the analytes may require a different method of introduction into the MS. Metals and metal ions may be introduced by HPLC if they are in solution but commonly are introduced via AAS or inductively coupled plasma (ICP). Other analytes may be directly introduced from HPLC to MS [2],... 

On the basis of the preceding discussion, it should be obvious that ultratrace elemental analysis can be performed without any major problems by atomic spectroscopy. A major disadvantage with elemental analysis is that it does not provide information on element speciation. Speciation has major significance since it can define whether the element can become bioavailable. For example, complexed iron will be metabolized more readily than unbound iron and the measure of total iron in the sample will not discriminate between the available and nonavailable forms. There are many other similar examples and analytical procedures that must be developed which will enable elemental speciation to be performed. Liquid chromatographic procedures (either ion-exchange, ion-pair, liquid-solid, or liquid-liquid chromatography) are the best methods to speciate samples since they can separate solutes on the basis of a number of parameters. Chromatographic separation can be used as part of the sample preparation step and the column effluent can be monitored with atomic spectroscopy. This mode of operation combines the excellent separation characteristics with the element selectivity of atomic spectroscopy. AAS with a flame as the atom reservoir or AES with an inductively coupled plasma have been used successfully to speciate various ultratrace elements. 

FIA star 5010 Modular, semi- or fully automatic operation. May be operated with process controller microprocessor. Can be set up in various combinations with 5017 sampler and superflow software which is designed to run on IBM PC/XT computer 60-180 samples h Dialysis for in-line sample preparation and in-line solvent extraction.Thermostat to speed up reactions. Spectrophotometer (400-700nm) or photometer can be connected to any flow through detector, e.g. UV/visible, inductively coupled plasma, atomic absorption spectrometer and ion-selective electrodes... 

Spectro- photometry Atomic absorption spectro- metry Inductively coupled plasma atomic emission spectrometry X-ray methods Ion selective electrodes Wet digestion methods Miscellaneous... 

An ion-selective electrode responds to the activity of free analyte, not complexed analyte. For example, when the Pb2+ in tap water at pH 8 was measured with a sensitive ion-selective electrode, the result was [Pb2+] = 2 X 10 10 M.25 When lead in the same tap water was measured by inductively coupled plasma-mass spectrometry (Section 21-6), the result was more than 10 times greater 3 X 10-9M. The discrepancy arose because the inductively coupled plasma measures all lead and the ion-selective electrode measures free Pb2+. In tap water at pH 8, much of the lead is complexed by CO -, OH, and other anions. When the pH of tap water was adjusted to 4, Pb2+ dissociated from its complexes and the concentration indicated by the ion-selective electrode was 3 X 10-9M—equal to that measured by inductively coupled plasma. 

The GECE sensors were used for lead determination in real water samples suspected to be contaminated with lead obtained from water suppliers. The same samples were previously measured by three other methods a potentiometric FIA system with a lead ion-selective-electrode as detector (Pb-ISE) graphite furnace atomic absorption spectrophotometry (AAS) inductively coupled plasma spectroscopy (ICP). The results obtained for lead determination are presented in Table 7.1. The accumulation times are given for each measured sample in the case of DPASV. Calibration plots were used to determine the lead concentration. GEC electrode results were compared with each of the above methods by using paired -Test. The results obtained show that the differences between the results of GECE compared to other methods were not significant. The improvement of the reproducibility of the methods is one of the most important issues in the future research of these materials. 

The nonsugar components in the hydrolysates were determined to be a collection of metals, anions, and nitrogenous material. The inorganic elements (Ca, K, Mg, Na, S, P, Al, Si) were measured by an inductively coupled plasma-optical emission spectrometer (ICP-OES). Dissolved ammonium was measured with an ion-selective electrode. 

Figure 14 Inductively coupled plasma mass spectra of a mixture of lanthanides, Y, and Th (a) without stored waveform inverse Fourier transform ion trap (SWIFT) excitation and (b) with the selective accumulation of Ce+ via SWIFT. (From Ref. 58.)...

Fig. 10. Schematic view of the Inductively-Coupled Plasma (ICP) Selected-Ion Flow Tube (SIFT) tandem mass spectrometer. The ICP torch produces metal ions M+ that are mass-selected and injected into the flow tube. The M+ ions may be ligated with molecules L before they enter the reaction region further downstream...

In both total and sequential dissolutions, the result is a solution containing the components of rocks and soils. This solution is then analyzed by different methods. Mostly, spectroscopic methods are used atomic absorption and emission spectroscopic methods, ultraviolet, atom fluorescence, and x-ray fluorescence spectrometry. Multielement methods (e.g., inductively coupled plasma optical emission spectroscopy) obviously have some advantages. Moreover, elec-troanalytical methods, ion-selective electrodes, and neutron activation analysis can also be applied. Spectroscopic methods can also be combined with mass spectrometry. 

Any type of detector with a flow-through cell can be used for FIA. Photometric detectors are most often used in FIA (15-18, 25). However, many other analyses using fluorimeters (28, 29), refractometers (24), atomic absorption (30, 31), and inductively coupled plasma emission spectrometers (32) have been described. Electrochemical detectors based on potentiometry with ion-selective electrodes (15, 33), anodic stripping voltammetry (15, 34), potentiometric stripping (35), and amperometry (36) have also been used. 

The most utilized methods include X-ray fluorescence (XRF), atomic absorption spectroscopy (AAS), activation analysis (AA), optical emission spectroscopy (OES) and inductively coupled plasma (ICP), mass spectroscopy (MS). Less frequently used techniques include ion-selective electrode (ISE), proton induced X-ray emission (PIXE), and ion chromatography (IC). In different laboratories each of these methods may be practiced by using one of several optional approaches or techniques. For instance, activation analysis may involve conventional thermal neutron activation analyses, fast neutron activation analysis, photon activation analysis, prompt gamma activation analysis, or activation analysis with radio chemical separations. X-ray fluorescence options include both wave-length and/or energy dispersive techniques. Atomic absorption spectroscopy options include both conventional flame and flameless graphite tube techniques. 

Milstein, L. S., Essader, A., Pellizzari, E. D., Fernando, R. A., Akinbo, O. Selection of a suitable mobile phase for the speciation of four arsenic compounds in drinking water samples using ion-exchange chromatography coupled to inductively coupled plasma mass spectrometry. Environ Int 2002, 28, 277-283. 

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