ATOMIC ABSORPTION-SPECTROMETRY 1 Technique

Willie et al. [17] used the hydride generation graphite furnace atomic absorption spectrometry technique to determine selenium in saline estuary waters and sea waters. A Pyrex cell was used to generate selenium hydride which was carried to a quartz tube and then a preheated furnace operated at 400 °C. Pyrolytic graphite tubes were used. Selenium could be determined down to 20 ng/1. No interference was found due to, iron copper, nickel, or arsenic. 

Ihnat M (1982) Application of Atomic Absorption Spectrometry to the Analysis of Foodstuffs. In Cantle JE, Ed. Atomic Absorption Spectrometry, Techniques and Instrumentation in Analytical Chemistry, Vol 5, Chap. 4d, pp. 139-210. Elsevier, Amsterdam. 

This study, still in progress, can serve as an example of using the atomic absorption spectrometry technique for the assistance, together with other techniques, in the clinical diagnosis of some diseases. 

Coker reported a gas chromatography/atomic absorption spectrometry technique for alkylleads in which he could analyze a sample in 5 min with a detection limit of 0.2 ppm lead, a value, he points out suitable for determining trace lead in unleaded gasoline. Alkyl-lead has recently been determined in the atmosphere with a GC-micro-wave plasma detector by Reamer et al. ... 

Highly sensitive iastmmental techniques, such as x-ray fluorescence, atomic absorption spectrometry, and iaductively coupled plasma optical emission spectrometry, have wide appHcation for the analysis of silver ia a multitude of materials. In order to minimize the effects of various matrices ia which silver may exist, samples are treated with perchloric or nitric acid. Direct-aspiration atomic absorption (25) and iaductively coupled plasma (26) have silver detection limits of 10 and 7 l-lg/L, respectively. The use of a graphic furnace ia an atomic absorption spectrograph lowers the silver detection limit to 0.2 l-ig/L. 

The complex of the following destmctive and nondestmctive analytical methods was used for studying the composition of sponges inductively coupled plasma mass-spectrometry (ICP-MS), X-ray fluorescence (XRF), electron probe microanalysis (EPMA), and atomic absorption spectrometry (AAS). Techniques of sample preparation were developed for each method and their metrological characteristics were defined. Relative standard deviations for all the elements did not exceed 0.25 within detection limit. The accuracy of techniques elaborated was checked with the method of additions and control methods of analysis. 

Figure 15-12 is a schematic illustration of a technique known as acid volatile sulfides/ simultaneously extracted metals analysis (AVS/SEM). Briefly, a strong acid is added to a sediment sample to release the sediment-associated sulfides, acid volatile sulfides, which are analyzed by a cold-acid purge-and-trap technique (e.g., Allen et ai, 1993). The assumption shown in Fig. 15-12 is that the sulfides are present in the sediments in the form of either FeS or MeS (a metal sulfide). In a parallel analysis, metals simultaneously released with the sulfides (the simultaneously extracted metals) are also quantified, for example, by graphite furnace atomic absorption spectrometry. Metals released during the acid attack are considered to be associated with the phases operationally defined as "exchangeable," "carbonate," "Fe and Mn oxides," "FeS," and "MeS."... 

The scope of this review Is limited to electrothermal atomic absorption spectrometry, with emphasis upon Its clinical applications. This article Is Intended to supplement the recent treatises on the basic technique which have been written by Aggett and Sprott ( ) > Ingle ( ), Klrkbrlght (34), Price (63), and Woodrlff (83). This resume does not consider various related topics, such as (a) atomic fluorescence or emission spectrometry (b) non-flame atomization devices which employ direct current... 

Metal ions are most commonly measured using atomic absorption spectrometry. In this technique... 

Atsuya I, Itoh K, Akatsuka K (1987) Development of direct analysis of powder samples by atomic absorption spectrometry using the inner miniature cup technique. Fresenius Z Anal Chem 328 338-341. 

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. 

Note that the interfacing of LC techniques with MS puts significant constraints on the solvents that can be used i.e., they must be volatile, with a low salt concentration, for MS compatibility. Narrow-bore columns, which use much smaller amounts of salt and organic modifier, appear to have potential for facilitating IEC-MS applications.40 Despite the excellent sensitivity of MS detection for most elements, however, there are cases where matrix effects can interfere. In this situation, combination of IEC with atomic emission spectrometry (AES) or atomic absorption spectrometry (AAS) may be preferable, and can also provide better precision.21 32 4142 Other types of... 

Principles and Characteristics Plasma source techniques are more widely used in connection with liquid chromatography than atomic absorption spectrometry (see Section 7.3.3). ICP is a natural complement to liquid chromatography, and HPLC-ICP procedures... 

It is an advantage of electroanalysis and its apparatus that the financial investment is low in comparison, for instance, with the more instrumental spectrometric methods real disadvantages are the need to have the analyte in solution and to be familiar with the various techniques and their electrochemistry it is to be regretted that the knowledge of chemistry and the skill needed often deter workers from applying electroanalysis when this offers possibilies competitive with more instrumental methods (cf., stripping voltammetry versus atomic absorption spectrometry). 

The low concentrations of lead in plasma, relative to red blood cells, has made it extremely difficult to accurately measure plasma lead concentrations in humans, particularly at low PbB concentrations (i.e., less than 20 pg/dL). However, more recent measurements have been achieved with inductively coupled mass spectrometry (ICP-MS), which has a higher analytical sensitivity than earlier atomic absorption spectrometry methods. Using this analytical technique, recent studies have shown that plasma lead concentrations may correlate more strongly with bone lead levels than do PbB concentrations (Cake et al. 1996 Hemandez-Avila et al. 1998). The above studies were conducted in adults, similar studies of children have not been reported. 

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. 

First step of the approach is the chemical characterization of leachate using well-established analytical techniques (Fig. 2) GC-MS for polar organic compounds (POCs), HRGC-MS for PCDD/Fs, PCBs and PAHs [18], atomic absorption spectrometry for heavy metals and ion chromatography for ammonia. 

Chapters 5 and 6 discuss the application of new techniques such as atomic absorption spectrometry with and without graphite furnace and Zeeman background correction, inductively coupled plasma mass spectrometry, X-ray fluo-... 

Mercury was determined after suitable digestion by the cold vapour atomic absorption method [40]. Lead was determined after digestion by a stable isotope dilution technique [41-43]. Copper, lead, cadmium, nickel, and cobalt were determined by differential pulse polarography following concentration by Chelex 100 ion-exchange resin [44,45], and also by the Freon TF extraction technique [46]. Manganese was determined by flameless atomic absorption spectrometry (FAA). 

The following analytical techniques seem to be adequate for the concentrations under consideration copper and nickel by Freon extraction and FAA cold vapour atomic absorption spectrometry, cobalt by Chelex extraction and differential pulse polarography, mercury by cold vapour atomic absorption absorptiometry, lead by isotope dilution plus clean room manipulation and mass spectrometry. These techniques may be used to detect changes in the above elements for storage tests Cu at 8 nmol/kg, Ni at 5 nmol/kg, Co at 0.5 nmol/kg, Hg at 0.1 nmol/kg, and Pb at 0.7 nmol/kg. 

A limited amount of work has been carried out on the determination of molybdenum in seawater by AAS [107-109] and graphite furnace atomic absorption spectrometry [110]. In a recommended procedure a 50 ml sample at pH 2.5 is preconcentrated on a column of 0.5 gp-aminobenzylcellulose, then the column is left in contact with 1 mol/1 ammonium carbonate for 3 h, after which three 5 ml fractions are collected. Finally, molybdenum is determined by AAS at 312.2 nm with use of the hot-graphite-rod technique. At the 10 mg/1 level the standard deviation was 0.13 xg. 

Measurement techniques that can be employed for the determination of trace metals include atomic absorption spectrometry, anodic stripping voltammetry, differential pulse cathodic stripping voltammetry, inductively coupled plasma atomic emission spectrometry, liquid chromatography of the metal chelates with ultraviolet-visible absorption and, more recently, inductively coupled plasma mass spectrometry. 

Many of the published methods for the determination of metals in seawater are concerned with the determination of a single element. Single-element methods are discussed firstly in Sects. 5.2-5.73. However, much of the published work is concerned not only with the determination of a single element but with the determination of groups of elements (Sect. 5.74). This is particularly so in the case of techniques such as graphite furnace atomic absorption spectrometry, Zeeman background-corrected atomic absorption spectrometry, and inductively coupled plasma spectrometry. This also applies to other techniques, such as voltammetry, polarography, neutron activation analysis, X-ray fluroescence spectroscopy, and isotope dilution techniques. 

In the determination of cadmium in seawater, for both operational reasons and ease of interpretation of the results it is necessary to separate particulate material from the sample immediately after collection. The dissolved trace metal remaining will usually exist in a variety of states of complexation and possibly also of oxidation. These may respond differently in the method, except where direct analysis is possible with a technique using high-energy excitation, such that there is no discrimination between different states of the metal. The only technique of this type with sufficiently low detection limits is carbon furnace atomic absorption spectrometry, which is subject to interference effects from the large and varying content of dissolved salts. 

In contrast, the coupling of electrochemical and spectroscopic techniques, e.g., electrodeposition of a metal followed by detection by atomic absorption spectrometry, has received limited attention. Wire filaments, graphite rods, pyrolytic graphite tubes, and hanging drop mercury electrodes have been tested [383-394] for electrochemical preconcentration of the analyte to be determined by atomic absorption spectroscopy. However, these ex situ preconcentration methods are often characterised by unavoidable irreproducibility, contaminations arising from handling of the support, and detection limits unsuitable for lead detection at sub-ppb levels. 

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