Elements of interest

To give the analyst some idea of the elemental content to be expected in foodstuffs, a listing of estimated typical ranges of some of the more important elements in 12 different classes of food is presented in Table 1. The data referring to total concentrations in edible food portions were distilled from the extensive compilations on Na, K, Mg, Ca, Fe and Zn in a vast variety of foods, contained in USDA Handbooks 8, 8-1 and 8-2 [65—67], the compilations for 12 trace elements authored by Schlettwein-Gsell and Mommsen-Straub [68, 69], and a number of other publications referred to in the Table [64a, 65—119]. Selection of elements considered in this chapter relates to Table 1. 

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In addition, the volume element of interest is not the box dx dy dz shown in Fig. 1.6a but, rather, a spherical shell of radius r and thickness dr as shown in Fig. 1.6b. The result of expressing the volume element in spherical coordinates and integrating over all angles is the replacement... 

For quantitative analysis, the resolution of the spectral analyzer must be significantly narrower than the absorption lines, which are - 0.002 nm at 400 nm for Af = 50 amu at 2500°C (eq. 4). This is unachievable with most spectrophotometers. Instead, narrow-line sources specific for each element are employed. These are usually hoUow-cathode lamps, in which a cylindrical cathode composed of (or lined with) the element of interest is bombarded with inert gas cations produced in a discharge. Atoms sputtered from the cathode are excited by coUisions in the lamp atmosphere and then decay, emitting very narrow characteristic lines. More recendy semiconductor diode arrays have been used for AAS (168) (see Semiconductors). 

A discussion of methods and appHcations for trace analysis of cosmetics is available (167). Analyses of elements from Al to Zn by a variety of methods has also been described recendy (168). Detection techniques for some of the elements of interest foUow ... 

Device A device is the smallest element of interest to batch logic. Examples of devices include measurement devices and actuators. 

The influenee of sodium and organie eomponent on analytieal signal values of elements of interest is investigated. ICP parameters (flow rate, power and inner injeetor diameter) are optimized. 

With the same scanning capability, it is much faster and often more useful to simply scan one line on a sample. The data is again output to a color CRT, but it is presented as the modulation of the y-amplitude, which is determined by the intensity of the X-ray signal production ftom the ROI of the element of interest. As the probe scans along the line, the CRT plots a graph of the elemental counting rates versus distance. Here again, it is usually possible to plot the data from many ele-... 

The results shown in Figure 6 above are an example of this mode of analysis, but include additional information on the chemical states of the Si. The third most frequently used mode of analysis is the Auger mapping mode, in which an Auger peak of a particular element is monitored while the primary electron beam is raster scanned over an area. This mode determines the spatial distribution, across the surface, of the element of interest, rather than in depth, as depth profiling does. Of course, the second and third modes can be combined to produce a three-dimensional spatial distribution of the element. The fourth operational mode is just a subset of the third mode a line scan of the primary beam is done across a region of interest, instead of rastering over an area. 

There are two major drawbacks to ISS concerning quantitative analysis. First, it has very low spectral resolution. Thus it is very difficult either to identify or resolve many common adjacent elements, such as Al/SI, K/Ca, and Cu/Zn. If the elements of interest are sufficiendy high in mass, this can be partially controlled by using a probe gas with a higher atomic mass, such as Ne or Ar. Second, ISS has an inherendy high spectral background which often makes it difficult to determine... 

An ICP-OES instrument consists of a sample introduction system, a plasma torch, a plasma power supply and impedance matcher, and an optical measurement system (Figure 1). The sample must be introduced into the plasma in a form that can be effectively vaporized and atomized (small droplets of solution, small particles of solid or vapor). The plasma torch confines the plasma to a diameter of about 18 mm. Atoms and ions produced in the plasma are excited and emit light. The intensity of light emitted at wavelengths characteristic of the particular elements of interest is measured and related to the concentration of each element via calibration curves. 

Calibration curves must be made using a series of standards to relate emission intensities to the concentration of each element of interest. Because ICP-OES is relatively insensitive to matrix effects, pure solutions containing the element of interest often are used for calibration. For thin films the amount of sample ablated by spark discharges or laser sources is often a strong function of the sample s composition. Therefore, either standards with a composition similar to the sample s must be used or an internal standard (a known concentration of one element) is needed. 

Direct-reading polychromators (Figure 3b) have a number of exit slits and photomultiplier tube detectors, which allows one to view emission from many lines simultaneously. More than 40 elements can be determined in less than one minute. The choice of emission lines in the polychromator must be made before the instrument is purchased. The polychromator can be used to monitor transient signals (if the appropriate electronics and software are available) because unlike slew-scan systems it can be set stably to the peak emission wavelength. Background emission cannot be measured simultaneously at a wavelength close to the line for each element of interest. For maximum speed and flexibility both a direct-reading polychromator and a slew-scan monochromator can be used to view emission from the plasma simultaneously. 

In recent years TOF SIMS has also proved to he a very powerful tool for ultra-shallow depth profiling, having the advantage of simultaneously detecting all elements of interest. The dual beam mode [3.41], in particular, (see Sect. 3.2.2.1) enables optimized depth resolution, because sputtering conditions can be independently optimized. 

The counting time for one pixel, and the number of pixels, determine the measurement time for one image. For low concentrations of the elements of interest the Pois-... 

Of the elements commonly found in lead alloys, zinc and bismuth aggravate corrosion in most circumstances, while additions of copper, tellurium, antimony, nickel, silver, tin, arsenic and calcium may reduce corrosion resistance only slightly, or even improve it depending on the service conditions. Alloying elements that are of increasing importance are calcium especially in maintenance-free battery alloys and selenium, or sulphur combined with copper as nucleants in low antimony battery alloys. Other elements of interest are indium in anodesaluminium in batteries and selenium in chemical lead as a grain refiner ". 

Minerals generally present difficult problems in chemical analysis, and these problems grow more serious when the elements being determined are as difficult to separate as are those named above. The time and effort that x-ray emission spectrography can save are therefore great, but there are obstacles to be surmounted. Among these are (1) Absorption and enhancement effects are often serious. (2) The element of interest may be present at low concentration in a matrix that is unknown and variable. (3) Satisfactory standards are not always easy to obtain. (4) Simple equipment sometimes does not resolve important analytical lines- completely. (5) Sample preparation and particle size often influence the intensities of analytical lines Class II deviations (7.8) can be particularly serious with minerals. 

Group I. Element of interest variable in a virtually constant matrix. 

Examples Fe and Mn in domestic ores.73 Group IV. One or more elements of interest in a variable matrix. 

Description of the cell composition is based - as far as possible - on the Stockholm convention (1953), i.e. the left-hand electrode constitutes the negative terminal of the cell. Cells are listed according to the metallic constituent of the electrode mentioned first which is involved in the electrode reaction establishing the respective electrode potential. Contact materials and conductive additives may be mentioned first before the actual element of interest only for the sake of correct materials sequence. The sequence of electrode components is stated as reported in the original publications. When an oxygen electrode is used as reference electrode an oxygen partial pressure of 0.21 atm is assumed. 

The primary consideration for all AEM analysis is that the specimen be thin (generally carbon coated electron microscope grid either dry or in a suitable liquid. If a liquid suspension is used in preparing the specimen, it is important that all elements of interest are insoluble in that liquid. Only particles thin enough to meet AEM thin-film criteria (15) should be analyzed quantitatively. Scraping surface particles from a catalyst pellet for specimen preparation may be more useful than grinding the entire pellet. 

The approach taken here is to use the lattice strain model to derive the partition coefficient of a U-series element (such as Ra) from the partition coefficient of its proxy (such as Ba) under the appropriate conditions. Clearly the proxy needs to be an element that forms ions of the same charge and similar ionic radius to the U-series element of interest, so that the pair are not significantly fractionated from each other by changes in phase composition, pressure or temperature. Also the partitioning behavior of the proxy must be reasonably well constrained under the conditions of interest. Having established a suitable partition coefficient for the proxy, the partition coefficient for the U-series element can then be obtained via rearrangement of Equation (2) (Blundy and Wood 1994) ... 

Although the need for complete decomposition is often stressed (see also Table 8.3), not all detection techniques demand the same degree of mineralisation. Table 8.6 classifies analytical techniques according to the amount of mineralisation that they need [4]. Ideally, a purely instrumental approach is the only way to prevent losses and contamination due to decomposition. Choosing a decomposition mode simply to be able to meet the requirements of the detection technique is an incomplete approach. The choice of decomposition should primarily be directed by both the matrix and element of interest. 

Principles and Characteristics Combustion analysis is used primarily to determine C, H, N, O, S, P, and halogens in a variety of organic and inorganic materials (gas, liquid or solid) at trace to per cent level, e.g. for the determination of organic-bound halogens in epoxy moulding resins, halogenated hydrocarbons, brominated resins, phosphorous in flame-retardant materials, etc. Sample quantities are dependent upon the concentration level of the analyte. A precise assay can usually be obtained with a few mg of material. Combustions are performed under controlled conditions, usually in the presence of catalysts. Oxidative combustions are most common. The element of interest is converted into a reaction product, which is then determined by techniques such as GC, IC, ion-selective electrode, titrime-try, or colorimetric measurement. Various combustion techniques are commonly used. 

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