Flame spectrometric detection

A flame spectrometric detection (FSD) system was used to study a variety of metal chelates including the UO(tfac)2, Cr(tfac)3, Cr(hfac)3, Al(tfac)3, Cu(tfac)2, Fe(hfac)2, Cu(hfac)2, Co(hfac)2 and tricarbonylchromium complexes. The GC column was connected by a heated stainless steel line to a flame spectrometer, working in a laminar flow regime with a N2O-C2H2 premix burner that could be heated without distortion of the flame, and a monochromator provided the selective response required for the FSD. The system included a splitter to allow simultaneous FID and FSD chromatograms . ... 

Atomic Absorption/Emission Spectrometry. Atomic absorption or emission spectrometric methods are commonly used for inorganic elements in a variety of matrices. The general principles and appHcations have been reviewed (43). Flame-emission spectrometry allows detection at low levels (10 g). It has been claimed that flame methods give better reproducibiHty than electrical excitation methods, owing to better control of several variables involved in flame excitation. Detection limits for selected elements by flame-emission spectrometry given in Table 4. Inductively coupled plasma emission spectrometry may also be employed. 

Amirav A, Jing H. 1998. Simultaneous pulsed flame photometric and mass spectrometric detection for enhanced pesticide analysis capabilities. J Chromatogr 814 133-150. 

Kugler, F. et ah. Determination of free amino compounds in betalainic fruits and vegetables by gas chromatography with flame ionization and mass spectrometric detection, J. Agric. Food Chem., 54, 4311, 2006. 

Krock and Wilkins [4] have used multidimensional gas chromatography with infrared and mass spectrometric detection to determine organics in soil. Direct acetylation followed by gas chromatography with flame ionization, electron capture and mass spectrometric detectors has been used to determine phenolic residues in soil [5]. Llopart-Visoso et al. [6] have used direct acetylation followed by headspace gas chromatography to determine phenolic and cresolic components of soil. 

Elimination of wet chemical sample preparation enables a complete analysis to be performed and data to be quickly analyzed. The detection limits are in the low part-per-million range using mass spectrometric detection. Alternatively, detection of compounds can be achieved by all common gas chromatography detectors (flame ionization detector, electron capture detector and flame photometric detector), and detection limits are determined by the method of detection employed. 

Capillary columns may provide the best method for the separation of phenols prior to their quantification (Eichelberger et al. 1983 Shafer et al. 1981 Sithole et al. 1986). Of the various methods available for detection, the two commonly used methods that are most sensitive are mass spectrometry and flame ionization detection. Although electron capture detectors provide good sensitivities for higher chlorine-substituted phenols, they are poor for phenol itself (Sithole et al. 1986). The best method for the quantification of phenol may be mass spectrometric detection in the selected ion mode, but the loss of qualitative information may be significant (Eichelberger et al. 1983). 

S. Cerutti, S. L. C. Ferreira, J. A. Gasquez, R. A. Olsina and L. D. Martinez, Optimisation of the preconcentration system of cadmium with 1 -(2-thiazolylazo)-7 -cresol using a knotted reactor and flame atomic absorption spectrometric detection, J. Hazard. Mater., 112(3), 2004, 279-283. 

Sperling, M., Xu, S. and Welz, B. (1992) Determination of chromium (III) and chromium (VI) in water using flow injection on-line preconcentration with selective adsorption on activated alumina and flame atomic absorption spectrometric detection. Anal. Chem., 64, 3101-3108. 

Matthias et al. [216] have described a comprehensive method for the determination of aquatic butyltin and butylmethyltin species at ultratrace levels using simultaneous sodium borohydride hydridisation, extraction with gas chromatography-flame photometric detection and gas chromatography-mass spectrometric detection. The detection limits for a lOOmL sample were 7ng L 1 of tin for tetrabutyltin and tributyltin, 3ng L 1 of tin for dibutyltin and 22ng L 1 tin for monobutyltin. For 800mL samples detection limits were l-2ng L 1 tin for tri- and tetrabutyltin and below lng L 1 tin for dibutyltin. The technique was applied to the detection of biodegradation products of tributyltin in non saline waters. 

B.A. Tomkins, G.A. Sega and C.-H. Ho, Determination of Lewisite oxide in soil using solid-phase microextraction followed by gas chromatography with flame photometric or mass spectrometric detection, J. Chromatogr., A, 909, 13-28 (2001). 

D.R. Killelea and J.H. Aldstadt, Solid-phase microextraction method for gas chromatography with mass spectrometric and pulsed flame photometric detection studies of organoasenical speciation, J. Chromatogr. A, 918, 169-175 (2001). 

The most sensitive flame spectrometric procedure for the determination of strontium is FES, the emission intensity at 460.7 nm being measured from a nitrous oxide-acetylene flame. A detection limit of 1 ng ml-1 or better is generally readily attainable, although the element has a low ionization potential and addition of potassium or caesium at a final concentration of 2-5 mg ml 1 is essential as an ionization buffer. Chemical interference from phosphate, silicate and aluminium is reduced dramatically in this flame. 

Detector Flame-ionization or mass spectrometric detection... 

With mass spectrometric detection. With flame-ionization detection. 

Choice of the proper detection scheme is dependent on the properties of the analyte. Different types of detectors are available such as ultraviolet (UV), fluorescence, electrochemical, hght scattering, refractive index (RI), flame ionization detection (FID), evaporative light scattering detection (ELSD), corona aerosol detection (CAD), mass spectrometric (MS), NMR, and others. However, the majority of reversed-phase and normal-phase HPLC method development in the pharmaceutical industry is carried out with UV detection. In this section the practical use of UV detection will be discussed. 

Direct nebulization of an aqueous or organic phase containing extracted analytes has been widely used in flame atomic absorption spectroscopy [69-72], inductively coupled plasma atomic emission spectrometry [73-76], microwave induced plasma atomic emission spectrometry [77-80] and atomic fluorescence spectrometry [81], as well as to interface a separation step to a spectrometric detection [82-85]. 

The conventional sensitive and specific GC detection such as electron-capture detector (BCD) (see Fig. 2), flame thermionic detector (FTD), and flame photometric detector (FPD) are still widely used in pesticide residue analysis. In recent years, mass spectrometric detection is becoming more and more important. Although other types of mass analyzers are commercially available, the equipment used in modern residue laboratories is based on two major types the classical quadrupole mass analyzers and those based on the ion trap (also called tridimensional quadrupole). 

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