Atomic emission spectrometry, lead analysis

ASTM. 1998a. ASTME1613. Standard test method for analysis of digested samples for lead by inductively coupled plasma atomic emission spectrometry (ICP-AES). Flame Atomic Absorption (FAAS), or Graphite Furnace Atomic Absorption (GFAA) Techniques. American Society for Testing and Materials. 

The determination of lead in soil is also discussed under Multi-Cation Analysis in Sects. 2.55 (inductively coupled plasma atomic emission spectrometry), 2.55 (atomic absorption spectrometry), 2.55 (photon activation analysis), 2.55 (emission spectrometry), 2.55 (anodic stripping voltammetry) and 2.55 (neutron activation analysis). 

Lobinski, R. and Adams, F.C. (1992a) Sensitive speciation analysis of lead in environmental waters by capillary gas chromatography microwave-induced plasma atomic emission spectrometry. Anal. Chim. Acta, 262, 285-297. 

The EPA mobile lab analyzed soil samples for lead, zinc, copper, and nickel by XRF. Because arsenic had been identified as the element that presents the greatest risk to human health at the Cos Cob site, samples from the 0—1 ft (0—0.3 m) to 1—2 ft (0.3-0.6 m) intervals were sent off-site for analysis by inductively coupled plasma/ atomic emission spectrometry. If the off-site analysis showed arsenic concentrations greater than 10 ppm (the Connecticut direct exposure criterion for soil), the field investigators progressively analyzed samples in 1 -ft (0.3 m) intervals below and surrounding the sample, delineating hot spots, until the remaining contamination was lower than 5 ppm. 

Ceulemans, M., Adams, F 1996. Integrated sample preparation and speciation analysis for simultaneous determination of methylated species of tin, lead and mercury in water by purge-and-trap injection-capillary gas chromatography - Atomic emission spectrometry. J. Anal. Atom. Spectrom. 11, 201-206. 

Trace metals present in foods can have nutritional or toxicological significance and in the case of certain metals, e.g., copper and zinc, both of these. Fruit products are routinely tested for trace metal contents, e.g., canned fruits for tin, iron, copper, and zinc fruit juices for copper, zinc, and lead tomato puree for copper and also lead, tin, and arsenic. Statutory limits exist for many metals, e.g., lead, arsenic, zinc, and copper. Atomic emission spectrometry is now widely used for trace metal analysis as multielement determinations can be made on a single sample however, other methodologies are... 

Adsorption capacities were studied -by Atomic Emission Spectroscopy (Vista-Pro ICP-OES from VARIAN) for lead analysis and -by UV Spectrometry (Nicolet Evolution 300 from ThermoElectron Corporation) for p-nitrophenol determination. 

In the analysis of solutions, pneumatic nebulization and then the introduction of the aerosol into the source are already well known from the early work on flame emission spectrometry. Pneumatic nebulizers must enable a fine aerosol to be produced, which leads to a high efficiency, and the gas flow used must be low enough to transport the droplets of the aerosol through the source with a low velocity. The production of fine droplets and the use of low gas flows are essential to obtaining complete atomization in the source. 

Atomization of the sample is usually facilitated by the same flame aspiration technique that is used in flame emission spectrometry, and thus most flame atomic absorption spectrometers also have the capability to perform emission analysis. The previous discussion of flame chemistry with regard to emission spectroscopy applies to absorption spectroscopy as well. Flames present problems for the analysis of several elements due to the formation of refractory oxides within the flame, which lead to nonlinearity and low limits of detection. Such problems occur in the determination of calcium, aluminum, vanadium, molybdenum, and others. A high-temperature acetylene/nitrous oxide flame is useful in atomizing these elements. A few elements, such as phosphorous, boron, uranium, and zirconium, are quite refractory even at high temperatures and are best determined by nonflame techniques (Table 2). 

The determination of trace metal impurities in pharmaceuticals requires a more sensitive methodology. Flame atomic absorption and emission spectroscopy have been the major tools used for this purpose. Metal contaminants such as Pb, Sb, Bi, Ag, Ba, Ni, and Sr have been identified and quantitated by these methods (59,66-68). Specific analysis is necessary for the detection of the presence of palladium in semisynthetic penicillins, where it is used as a catalyst (57), and for silicon in streptomycin (69). Furnace atomic absorption may find a significant role in the determination of known impurities, due to higher sensitivity (Table 2). Atomic absorption is used to detect quantities of known toxic substances in the blood, such as lead (70-72). If the exact impurities are not known, qualitative as well as quantitative analysis is required, and a general multielemental method such as ICP spectrometry with a rapid-scanning monochromator may be utilized. Inductively coupled plasma atomic emission spectroscopy may also be used in the analysis of biological fluids in order to detect contamination by environmental metals such as mercury (73), and to test serum and tissues for the presence of aluminum, lead, cadmium, nickel, and other trace metals (74-77). 

BIOLOGICAL PROPERTIES the biological half-life for lead in the bones of humans is 10 yrs can be detected in water by atomic adsorption or by colorimetric analysis or by inductively coupled plasma optical emission spectrometry, dissolved lead by 0.45 micron filtration prior to such analysis... 

This field provides a brief description of the suggested monitoring and analysis method for quantitative determination of a particular substance. For example, a method for quantitative determination has been developed for cadmium, copper, manganese, and lead in water by means of co-precipitation with zirconium hydroxide followed by subsequent analysis by atomic adsorption spectrometry. An Inductively Coupled Plasma-Atomic Emission Spectrophotometric method has been employed by the Environmental Protection Agency (EPA Method 200.7) for the determination of dissolved, suspended, or total elements in drinking water, surface water, and domestic and industrial wastewaters. 

Atomic absorption spectrometry (AAS) was established as the most popular gas chromatography (GC) detection technique for lead speciation analysis in the first years of speciation studies. The increase of the residence time of the species in the flame using a ceramic tube inside the flame and, later, the use of electrically heated tubes, made out of graphite or quartz where electrothermal atomization was achieved, provided lower detection limits but still not sufficiently low. Later, the boom of plasma detectors, mainly microwave induced plasma atomic emission (MIP-AES) and, above all, inductively coupled plasma atomic emission and mass spectrometry (ICP-AES and ICP-MS, respectively) allowed the sensitivity requirements for reliable organolead speciation analysis in environmental and biological samples (typically subfemtogram levels) to be achieved. These sensitivity requirements makes speciation analysis of organolead compounds by molecular detection techniques such as electrospray mass spectrometry (ES-MS) a very difficult task and, therefore, the number of applications in the literature is very limited. 

There are many analytical techniques which may be used for lead analysis. These include X-ray fluorescence (XRF) spectroscopy, radioactivation methods, emission spectrography, ring oven methods, polarographic techniques [including anodic stripping voltammetry (ASV)], spark source mass spectrometry, colorimetry and atomic absorption spectrometry (AAS). Background information upon all of these methods may be found in the Handbook of Air Pollution Analysis [1]. 

Field measurement of bulk soil lead by XRF instruments will typically require confirmation analysis through some randomly selected subset of further testing by some reference technique in the laboratory A AS, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), or ICP-mass spectrometry (ICP-MS). Other methods are electrochemical in nature, such as ASV and differential pulse polarography. Many soil samples are processed and analyzed directly in the laboratory. 

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