Spectrometry flame atomic absorption

It is easy to find a method for most types of matrices and the element of interest in standard methods publication, such as those from the American 

Society for Testing and Material (ASTM), US Environmental Protection Agency (USEPA), International Organisation for Standardisation (ISO), European Committee for Standardisation (CEN), Standard Methods for Water and Wastewater and Deutsches Institut fur Normung (DIN). 

But there is no specific FAAS standard method specially evaluated or approved for polluted soil samples there is the EPA methods (SW-846 EPA (2000)) or one ISO standard (ISO 11047). This standard is connected with the determination of several metals in aqua regia extracts. It provides a method for the determination of Cd, Cu, Co, Pb, Mn, Ni and Zn by flame and electrothermal atomic absorption spectrometric methods. 

To summarise, FAAS is very easy to use. Interferences are known and can be controlled. Extensive application information is also readily available. Its precision makes it an excellent technique for the determination of a number of commonly analysed elements at higher concentration in polluted soil samples. Its main drawback is its speed in relation to multi-element techniques such as ICP-AES and ICP-MS. Where direct-aspiration flame atomic absorption technique does not provide adequate sensitivity, reference is made to specialised techniques (in addition to graphite furnace procedure) such as the gaseous-hydride method for arsenic, antimony and selenium and the cold-vapour technique for mercury. 

Sensitivity is a term used in atomic absorption spectrometry to indicate the concentration that will cause an absorption of 1% (= 0.0044 absorbance units) of the hollow cathode resonance line radiation used for the determination. An example of typical instrumental sensitivity and detection limits for commercially available instruments is given in Table 4.3. 

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Cobalt and cobalt compounds in air Lab method using flame atomic absorption spectrometry 30/2... 

Koscielniak, R, Non-linear Robust Regression Procedure for Calibration in Flame Atomic Absorption Spectrometry, Analytica Chimica Acta 278, 1993, 177-187. 

Cruz, R. B. and Loon, J. C. van "A Critical Study of the Application of Graphite-Furnace Non-Flame Atomic Absorption Spectrometry to the Determination of Trace Base Metals In Complex Heavy-Matrix Sample Solutions". Anal. Chlm. Acta (1974), 72, 231-243. 

Flame atomic absorption spectrometry Flame emission spectrometry... 

Zhang D-Q, Li C-U, Yang L-L, Sun H-W (1998) Determination of cadmium in vegetables by derivative flame atomic absorption spectrometry with atom trapping technique. J Anal At Spectrom 13 1155-1158. 

Eaton AD, Clesceri LS, Greenberg AE. 1995b. Method 3111, Metals by Flame Atomic Absorption Spectrometry, Standard Methods for the Examination of Water and Wastewater, American Public Health Association, Washington, DC. 

Ho M.D., Evans G.J. Operational speciation of cadmium, copper, lead and zinc in the NIST standard reference materials 2710 and 2711 (Montana soil) by the BCR sequential extraction procedure and flame atomic absorption spectrometry. Anal Commun 1997 34 353-364. 

Other methods reported for the determination of beryllium include UV-visible spectrophotometry [80,81,83], gas chromatography (GC) [82], flame atomic absorption spectrometry (AAS) [84-88] and graphite furnace (GF) AAS [89-96]. The ligand acetylacetone (acac) reacts with beryllium to form a beryllium-acac complex, and has been extensively used as an extracting reagent of beryllium. Indeed, the solvent extraction of beryllium as the acety-lacetonate complex in the presence of EDTA has been used as a pretreatment method prior to atomic absorption spectrometry [85-87]. Less than 1 p,g of beryllium can be separated from milligram levels of iron, aluminium, chromium, zinc, copper, manganese, silver, selenium, and uranium by this method. See also Sect. 5.74.9. 

Armannsson [659] has described a procedure involving dithizone extraction and flame atomic absorption spectrometry for the determination of cadmium, zinc, lead, copper, nickel, cobalt, and silver in seawater. In this procedure 500 ml of seawater taken in a plastic container is exposed to a 1000 W mercury arc lamp for 5-15 h to break down metal organic complexes. The solution is adjusted to pH 8, and 10 ml of 0.2% dithizone in chloroform added. The 10 ml of chloroform is run off and after adjustment to pH 9.5 the aqueous phase is extracted with a further 10 ml of dithizone. The combined extracts are washed with 50 ml of dilute ammonia. To the organic phases is added 50 ml of 0.2 M-hydrochloric acid. The phases are separated and the aqueous portion washed with 5 ml of chloroform. The aqueous portion is evaporated to dryness and the residue dissolved in 5 ml of 2 M hydrochloric acid (solution A). Perchloric acid (3 ml) is added to the organic portion, evaporated to dryness, and a further 2 ml of 60% perchloric acid added to ensure that all organic matter has been... 

Fang et al. [661] have described a flow injection system with online ion exchange preconcentration on dual columns for the determination of trace amounts of heavy metal at pg/1 and sub-pg/1 levels by flame atomic absorption spectrometry (Fig. 5.17). The degree of preconcentration ranges from a factor of 50 to 105 for different elements, at a sampling frequency of 60 samples per hour. The detection limits for copper, zinc, lead, and cadmium are 0.07, 0.03, 0.5, and 0.05 pg/1, respectively. Relative standard deviations are 1.2-3.2% at pg/1 levels. The behaviour of the various chelating exchangers used was studied with respect to their preconcentration characteristics, with special emphasis on interferences encountered in the analysis of seawater. 

Cabezon et al. [662] simultaneously separated copper, cadmium, and cobalt from seawater by coflotation with octadecylamine and ferric hydroxide as collectors prior to analysis of these elements by flame atomic absorption spectrometry. The substrates were dissolved in an acidified mixture of ethanol, water, and methyl isobutyl ketone to increase the sensitivity of the determination of these elements by flame atomic absorption spectrophotometry. The results were compared with those of the usual ammonium pyrrolidine dithiocarbamate/methyl isobutyl ketone extraction method. While the mean recoveries were lower, they were nevertheless considered satisfactory. 

Tony et al. [951] have discussed an online preconcentration flame atomic absorption spectrometry method for determining iron, cobalt, nickel, magnesium, and zinc in seawater. A sampling rate of 30 samples per hour was achieved and detection limits were 4.0,1.0,1.0,0.5, and 0.5 xg/l, for iron, cobalt, nickel, magnesium, and zinc, respectively. 

Practical system for flame atomic absorption spectrometry including a deuterium background corrector. 

Flame atomic absorption spectrometry has achieved very wide use as a routine method for the determination of trace metals in solution. However, for alkali metals flame photometry has remained popular. Why is this ... 

Total dissolved Fe and Mn were analyzed directly by flame atomic absorption spectrometry (AAS). As was measured by AAS with hydride generation (HG-FIAS). Total dissolved Se concentrations were determined by hydride-generation atomic fluorescence spectrometry (Chen etal., 2005). 

Klenke et al. [5] described a technique for extraction of humic and fulvic acids from stream sediments and outlined methods for their determination. By means of flame atomic absorption spectrometry, the levels of environmentally important heavy metals (cadmium, copper, chromium, cobalt, nickel and lead) in the fulvic and humic acid extracts were compared with those in the original sediment samples. The pattern distribution of the respective metals in the two cases showed very close agreement, suggesting that the combined extract of humic and fulvic acids could be used as an indicator of the level of heavy metal pollution in flowing waters. 

Thiocyanate Human serum, urine, saliva Extraction of buffered (pH 7) 2-benzoyl pyridine thiosemi-carbazone and sample with isoamyl acetate Flame atomic absorption spectrometry 4 ng/mL 96-102 Chattaraj and Das 1992... 

An analyte transport efficiency of nearly 100% has been obtained with an interface for flame atomic absorption spectrometry (FAAS) [3]. It has been used for the determination of lead in blood [5] and for coupHng with a high-performance Hquid chromatograph (HPLC) [6]. 

A number of applications of flow-injection techniques have been made to flame atomic absorption spectrometry [22]. Although manifolds can be connected directly to the nebuhzer, the response of the spectrometer is dependent on the flow rate of the sample into the nebuhzer [23], and some adjustment to the manifold may be required. The optimum flow rate for maximum response when the sample enters the nebuhzer as a discrete sample plug can be different from that found for analysis of a continuous sample stream. 

If refers to flame atomic absorption spectrometry and NF to flameless atomic absorption spectrometry (e.g. carbon rod). 

Flame Atomic Absorption Spectrometry—Analytical Methods, Varian Publication No. 85-100 009-00, Varian Australia, Mulgrave, 1989, p. 35. 

Molybdenum may be identified at trace concentrations by flame atomic absorption spectrometry using nitrous oxide-acetylene flame. The metal is digested with nitric acid, diluted and analyzed. Aqueous solution of its compounds alternatively may be chelated with 8—hydroxyquinobne, extracted with methyl isobutyl ketone, and analyzed as above. The metal in solution may also be analyzed by ICP/AES at wavelengths 202.03 or 203.84 nm. Other instrumental techniques to measure molybdenum at trace concentrations include x-ray fluorescence, x-ray diffraction, neutron activation, and ICP-mass spectrometry, this last being most sensitive. 

These vitamers are UV absorbers, but their detection is complicated by the low level present in foods and the low sensitivity of this detector. Other detectors, like flame atomic absorption spectrometry and inductively coupled plasma (1CP)-MS, may be applied, but without much increase in sensitivity. 

Lei et al. reported a method for the indirect determination of trace amounts of procaine in human serum by atomic absorption spectrophotometry [54], The sample was mixed with HCIO4, heated at 85°C for 30 minutes, diluted to a known volume with water, and centrifuged. 1 mL of the supernatant solution was buffered with 0.1 M sodium acetate-acetic acid to pH 3.86, and mixed with 0.2 M Zn(SCN)j reagent to a final concentration of 0.1 M. After dilution to 50 mL with water, the solution was shaken for 1 minute with 10 mL of 1,2-dichloroethane, whereupon the zinc extracted into the organic phase was determined by air-acetylene flame atomic absorption spectrometry for the indirect determination of procaine. The detection limit was found to be 0.1 pg/g, with a recovery of 89-98% and a coefficient of variation (n = 10) equal to 3.2%. 

Table 2.2 Limits of detection for flame atomic absorption spectrometry...

Flame atomic absorption spectrometry can be used to determine trace levels of analyte in a wide range of sample types, with the proviso that the sample is first brought into solution. The methods described in Section 1.6 are all applicable to FAAS. Chemical interferences and ionization suppression cause the greatest problems, and steps must be taken to reduce these (e.g. the analysis of sea-water, refractory geological samples or metals). The analysis of oils and organic solvents is relatively easy since these samples actually provide fuel for the flame however, build-up of carbon in the burner slot must be avoided. Most biological samples can be analysed with ease provided that an appropriate digestion method is used which avoids analyte losses. 

An interesting application of speciation is in the study of changes in the distribution of certain metals after administration of drugs. Falchuk used gel filtration combined with flame atomic absorption spectrometry to study effects of the administration of ACTH on the zinc distribution in serum. Kamel et ai. developed methods to follow the distribution of gold. 

Flame atomic absorption spectrometry (FAAS) can be used to detect most elements present at levels greater than about 100 pg 1 . For more sensitive determinations graphite furnace atomic absorption spectrometry (GFAAS) is the technique of choice. In addition, if the volume of the fraction is limited GFAAS is ideally suited for the determination because only a few microfitres (5-20 pi) of sample... 

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