Spectroscopic elemental analysis emission method

Emission spectroscopy is the analysis, usually for elemental composition, of the spectmm emitted by a sample at high temperature, or that has been excited by an electric spark or laser. The direct detection and spectroscopic analysis of ambient thermal emission, usually ia the iafrared or microwave regioas, without active excitatioa, is oftea termed radiometry. la emission methods the sigaal iateasity is directiy proportioaal to the amouat of analyte present. 

As well as the atomic spectroscopic methods of flame photometry and atomic absorption spectroscopy microwave emission spectroscopic detection (MED) is being used more and more. MED combines high sensitivity in the picogram range with high selectivity for elemental analysis. It is as suitable for inorganic and organic compounds... 

More common methods for elemental analysis - to determine the elemental contents of a sample - include spectroscopy and spectrometry. Spectroscopy measures changes in atoms that cause a specific light photon to be either absorbed (absorption spectroscopy) or emitted (emission spectroscopy). This light has a precise wavelength or energy, characteristic of a specific element in the periodic table. The simplest (and oldest) form of elemental analysis was not spectroscopic, in fact, but colorimetric. This method was based on the reaction of a strongly colored chemical in a solution. The appearance of a specific color in the solution revealed the identity of the element of interest. If the color intensity is proportional to the amount of that element present, the method can also be used to estimate the amount of the element present. 

Atomic absorption spectroscopy (AAS) and flame emission spectroscopy (FES), also called flame photometry, are two analytical measurement methods relying on the spectroscopic processes of excitation and emission. Methods of quantitative analysis only, they are used to measure of around seventy elements (metal or non-metal). Many models of these instruments allow measurements to be conducted by these two techniques although their functioning principles are different. There exists a broad range of applications, as concentrations to the gtg/L (ppb) level can be accessed for certain elements. 

H. G. J. Moseley, Phil. Mag. [6], 26, 1024 (1913). The following remarkable quotation from this paper (p. 1030) supports Moseley as the founder of x-ray emission spectrography The prevalence of lines due to impurities suggests that this may prove a powerful method of chemical analysis. Its advantage over ordinary spectroscopic methods lies in the simplicity of the spectra and the impossibility of one substance masking the radiation from another. It may even lead to the discovery of missing elements, as it will be possible to predict the position of their characteristic lines. ... 

Owing to their superior fluorescent yield, heavy elements ordinarily yield considerably more intense XRF bands than the light elements. This feature can be exploited to determine the concentration of inorganic species in a sample, or the concentration of a compound that contains a heavy element in some matrix. Many potential XRF applications have never been developed owing to the rise of atomic spectroscopic methods, particularly inductively coupled plasma atomic emission spectrometry [74]. Nevertheless, under the right set of circumstances, XRF analysis can be profitably employed. 

The element may be analyzed in aqueous acidified phase by flame and furnace atomic absorption, ICP emission and ICP-MS spectroscopic methods. Also, at trace concentrations the element may be measured by x-ray fluorescence and neutron activation analysis. Wavelength for AA measurement is 240.7 nm and for ICP analysis is 228.62 nm. 

Elemental composition H 1.56%, Te 98.44%. The gas is identified by its physical properties and measured by chemical analysis. Two most confirmatory methods recommended here are (1) GC/MS, the characteristic mass ions should be in the range 126 to 132, and (2) furnace-AA or ICP emission spectroscopic analysis for metalic tellurium. For the AA analysis, hydrogen telluride gas should be passed through water and the solution acidified and analyzed for tellurim. Hydrogen may be measured by the classical combustion method involving oxidation to form water, followed by gravimetry. 

Alternating or direct current arcs and spark discharge are common methods of excitation for emission spectroscopic analysis of rare earth elements. Emission spectra of rare earth elements contain a large number of lines. The three arbitrary groups are (i) spectra of La, Eu, Yb, Lu and Y, (ii) more complicated spectra of Sm, Gd and Tm, (iii) even more complicated spectra of Ce, Nd, Pr, Tb, Dy and Er. Rare earths have been analyzed with spectrographs of high resolution and dispersion up to 2 A/mm. Some salient information is presented in Table 1.36. 

Dalton TP, Li Q, Bittel D, Liang L, Andrews GK (1996) Oxidative stress activates metal-responsive transcription factor-1 binding activity. Occupancy in vivo of metal response elements in the metallothionein-I gene promoter. J Biol Chem 271 26233-26241 Danscher G, Howell G, Perez-Clausell J, Hertel N (1985) The dithizone, Timm s sulphide silver and the selenium methods demonstrate a chelatable pool of zinc in CNS. A proton activation (PIXE) analysis of carbon tetrachloride extracts from rat brains and spinal cords intravitally treated with dithizone. Histochemistry 83 419 22 Danscher G, Jensen KB, Frederickson CJ, Kemp K, Andreasen A, Juhl S, Stoltenberg M, Ravid R (1997) Increased amount of zinc in the hippocampus and amygdala of Alzheimer s diseased brains a proton-induced X-ray emission spectroscopic analysis of cryostat sections from autopsy material. J Neurosci Methods 76 53-59... 

Official Methods of Analysis of AOAC International, 17th edn. Rev 1, AOAC International, Gaithersburg, MD, USA, Official Method 985.01. Metals and Other Elements in Plants and Pet Foods - Inductively Coupled Plasma Emission Spectroscopic Method (2002)... 

Chapter 11 details the relevant methods of analysis for both metals and organic compounds. For elemental (metal) analysis, particular attention is given to atomic spectroscopic methods, including atomic absorption and atomic emission spectroscopy. Details are also provided on X-ray fluorescence spectrometry for the direct analysis of metals in solids, ion chromatography for anions in solution, and anodic stripping voltammetry for metal ions in solution. For organic compounds,... 

Accuracy and Precision. The accuracy and precision required of an atomic-emission spectroscopic method affect the approach used in the analysis as well as the time involved. A qualitative analysis requires a minimum of effort, but as better accuracy and precision are demanded, increasing care is needed. Even if a representative sample has been obtained, errors inherent in the method, human errors, and random errors contribute to inaccuracies. Spectrochemical equipment is largely responsible for the random errors that influence precision, and both method and individual laboratory errors influence the accuracy. In addition, relative precision and accuracy depend upon concentration levels. The standard deviation increases with increasing concentration, but the relative standard deviation decreases the latter may vary from a few percent to less than one percent using photographic detection, depending on the element and the concentration. 

Analytical methods of atomic spectroscopy have been used in forestry and wood product research since their earliest development. Nowadays, almost all of the spectroscopic techniques available are employed in the analysis of metals and trace elements in diverse samples of industrial and environmental origin. The techniques that find most regular application include flame atomic absorption spectroscopy (F-AAS), graphite furnace atomic absorption spectroscopy (GF-AAS), inductively coupled plasma atomic emission spectroscopy (ICP-AES) and, occasionally, also direct current plasma atomic emission spectroscopy (DCP-AES). In many applications F-AAS is a sufficiently sensitive and precise technique however, in the analysis of some environmental samples for trace elements (forest soils, plant material and water) where concentrations may be very low (of the order of 100 ng mL" ) the greater sensitivity of GF-AAS and ICP/DCP-AES is required. In considering the applications of atomic spectroscopy to forestry and... 

---