Spectroscopy inductively coupled argon plasma

Aluminum is best detected quaUtatively by optical emission spectroscopy. SoHds can be vaporized direcdy in a d-c arc and solutions can be dried on a carbon electrode. Alternatively, aluminum can be detected by plasma emission spectroscopy using an inductively coupled argon plasma or a d-c plasma. Atomic absorption using an aluminum hoUow cathode lamp is also an unambiguous and sensitive quaUtative method for determining alurninum. 

Numerous methods have been pubUshed for the determination of trace amounts of tellurium (33—42). Instmmental analytical methods (qv) used to determine trace amounts of tellurium include atomic absorption spectrometry, flame, graphite furnace, and hydride generation inductively coupled argon plasma optical emission spectrometry inductively coupled plasma mass spectrometry neutron activation analysis and spectrophotometry (see Mass spectrometry Spectroscopy, optical). Other instmmental methods include polarography, potentiometry, emission spectroscopy, x-ray diffraction, and x-ray fluorescence. 

The classical wet-chemical quaUtative identification of chromium is accompHshed by the intense red-violet color that develops when aqueous Cr(VI) reacts with (5)-diphenylcarba2ide under acidic conditions (95). This test is sensitive to 0.003 ppm Cr, and the reagent is also useful for quantitative analysis of trace quantities of Cr (96). Instmmental quaUtative identification is possible using inductively coupled argon plasma—atomic emission spectroscopy... 

Alcohol sulfates and alcohol ether sulfates separated by HPLC on a styrene-divinylbenzene copolymer column with 4 1 (v/v) methanol and 0.05 M ammonium acetate aqueous solution as the mobile phase were analyzed by simultaneous inductively coupled argon plasma vacuum emission spectroscopy (IPC), monitoring the 180.7-nm sulfur line as a sulfur-specific detector [294]. This method was applied to the analysis of these surfactants in untreated wastewaters. 

Gunn et al. [44] described the apphcation of a graphite-filament electrothermal vaporization apparatus as a sample introduction system for optical emission spectroscopy with an inductively coupled argon plasma source. Good detection levels were reported for the elements, and details of the interfacing requirements between the ICP and the graphite filament were explored. 

An alternative approach is to analyze the samples using procedures or instrumentation that will give the maximum amount of data for each sample. For example, recent advances in atomic spectroscopy, i.e., inductively coupled argon plasma emission spectroscopy (ICP-AES), allow 20 to 30 elements to be detected simultaneously. 

Actinide metal samples are characterized by chemical and structure analysis. Multielement analysis by spark source mass spectrometry (SSMS) or inductively coupled argon plasma (ICAP) emission spectroscopy have lowered the detection limit for metallic impurities by 10 within the last two decades. The analysis of O, N, H by vacuum fusion requires large sample, but does not distinguish between bulk and surface of the material. Advanced techniques for surface analysis are being adapted for investigation of radioactive samples (Fig. 11) ... 

Finally, we note that the photocorrosion process is strongly pH-dependent, occurring most readily in strongly acid solutions, and that the presence of a carboxylic acid is required for the occurrence of severe photocorrosion. In Table II we present analytical results, based on inductively coupled argon plasma (ICP) emission spectroscopy, for representative electrolyte solutions after 6-8 hr. of photo-Kolbe electrolysis with n-SrTiC anodes. It can be seen that the formation of soluble strontium and titanium species is... 

A variety of tests (ASTM D-1026, D-1262, D-1318, D-1368, D-1548, D-1549, D-2547 D-2599, D-2788, D-3340, D-3341, and D-3605) have been designated for the determination of metals in petroleum products. Determination of metals in whole feeds can be accomplished by combustion of the sample so that only inorganic ash remains. The ash can then be digested with an acid and the solution examined for metal species by atomic absorption (AA) spectroscopy or by inductively coupled argon plasma (ICP) spectrometry. 

Inductively coupled argon plasma emission spectrophotometry (ASTM D-5708) has an advantage over atomic absorption spectrophotometry (ASTM D-4628, ASTM D-5863) because it can provide more complete elemental composition data than the atomic absorption method. Flame emission spectroscopy is often used successfully in conjunction with atomic absorption spectrophotometry (ASTM D-3605). X-ray fluorescence spectrophotometry (ASTM D-4927, ASTM D-6443) is also sometimes used, but matrix effects can be a problem. 

Inductively coupled plasma (ICP) emission techniques can be used to measure selenium concentrations in air. ICP techniques offer multielement capabilities, but instrumentation is costly and background interference can be a problem (Koirtyohann and Morris 1986). The NIOSH-recommended method for determining selenium in air is inductively coupled argon plasma atomic emission spectroscopy (NIOSH... 

Spectral methods (spark source mass spectrometry SSMS, secondary ion mass spectrometry SIMS, inductively coupled argon plasma for emission spectroscopy ICAP-ES) which avoid separation steps are increasingly applied for multi-element analysis. Hot extraction is used for 0, N, H determinations. Oxygen is also determined by activation analysis, nitrogen after adaptation of classical methods (micro-Kjeldahl). Combination and comparison of different, independent methods are desirable, but hampered by the often limited availability of samples of actinides. 

Dube, P. (1988). Automated direct determination of copper in urine and whole blood by Zeeman-corrected atomic absorption spectrometry. Atomic Spectrosc., 2, 55-58 Fell, G.S., Smith, H., Howie, R.A. (1968). Neutron activation analysis for copper in biological material applied to Wilson s disease, J. Clin. Path., 21, 8-11 Gonsior, B., and Roth, M. (1983) Trace element analysis by particle and photon-induced X-ray emission spectroscopy, Talanta, 385-400 Hartley, T.F. and Ellis, D.J. (1972). Combined electrolysis and atomic absorption for the determination of copper in biological materials, Proc. Soc. Anal. Chem., 2, 281 Herber, R.F.M., Pieters. H.J.. and Elgersma, J.W., (1982). A comparison of inductively coupled argon plasma atomic emission spectrometry and electrothermal atomization atomic absorption spectrometry in the determination of copper and zinc in serum, Fresenius Z. Anal. Chem., 313.103-107... 

Inductively coupled plasma-atomic emission spectroscopy (ICP-AES) is used for multi-element determinations in blood and tissue samples. Detection in urine samples requires extraction of the metals with a polydithiocarbamate resin prior to digestion and analysis (NIOSH 1984a). Other satisfactory analytical methods include direct current plasma emission spectroscopy and determination by AAS, and inductively coupled argon plasma spectroscopy-mass spectrometry (ICP-MS) (Patterson et al. 1992 Shaw et al. 1982). Flow injection analysis (FIA) has been used to determine very low levels of zinc in muscle tissue. This method provides very high sensitivity, low detection limits (3 ng/mL), good precision, and high selectivity at trace levels (Fernandez et al. 1992b). 

HCI = hydrochloric acid HNO3 = nitric acid ICP = inductively coupled argon plasma spectroscopy KNO3 = potassium nitrite MIBK = methyl isobutyl ketone NAA = neutron activation analysis NH 4HCO3-DTPA = ammonium bicarbonate-diethyl enetriaminepentaacetic acid NR = not reported... 

Variations of the AAS technique are commonly used to detect zinc levels in air, water, and soil samples, as well as in certain plant and food samples. Inductively coupled argon plasma spectroscopy (ICP) is a recommended test method for analyzing solid waste samples to measure zinc. Using either the ICP method or the AAS method, operators of hazardous waste management facilities can determine whether a given sample is hazardous, based on the level of zinc in a sample of solid waste leachate. 

Inductively-Coupled Argon-Plasma Atomic Emission Spectroscopy (ICAP AES) 2.0 Any matrix NIOSH (1984A). Requires extensive sanple preparation and concentration of metal with chelating resin. Advantage is simultaneous analyses for as many as 10 metals from 1 sample. 

The buildup of soluble corrosion products can be used to monitor corrosion kinetics. This method has been used extensively in oil field corrosion inhibitor testing, particularly in sweet (CO2) systems with only small amounts of HjS present [29]. Iron analysis in the laboratory is most rapidly done on the bench with the Hach method (Phenantridine) [.30], although a host of other wet chemical methods are applicable. Instrumental methods include Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Argon Plasma Spectroscopy (ICAP). While both these methods are well suited for high volume routine analysis, care must be taken that the samples are not contaminated by even traces of hydrocarbons. This includes soluble hydrocarbons such as methanol, chelating compounds such as EDTA, or scale inhibition products. Also used in the laboratory is Ion Chromatography (IC). This latter method is even more sensitive to sample composition and not recommended on a routine basis. 

The concentration of inorganic components in forage crops varies according to crop maturity, temperature, and soil pH and composition. The analyses of mineral content can reveal soil or management deficiencies as well as optimum harvest time for proper crop management. Actual mineral analyses are used to determine the amount of mineral supplementation to be added to an animal ration for proper nutritional balance. Reference methods of analysis include inductively coupled argon plasma (ICP), atomic absorption spectroscopy (AAS), and x-ray fluorescence spectroscopy (XRF). These techniques are well established for the analysis of mineral elements in whole-plant material. The exact procedures for sample preparation and analysis are well documented. Copies of the procedures may be obtained from instrument manufacturers or are readily found using basic texts for each analytical technique. 

Inductively coupled argon plasma 6 000 to 8 000 Emission Inductively coupled plasma spectroscopy, ICP... 

The development of many alternative plasma sources has led to a resurgence of analytical atomic emission spectroscopy in recent years. The major plasma emission sources used for gas chromatographic detection have been the microwave-induced helium plasma, under atmospheric or reduced pressure (MIP), and the DC argon plasma (DCP). The inductively coupled argon plasma (ICP) has been used much less for GC than as an HPLC detector [4]. 

The section on Spectroscopy has been retained but with some revisions and expansion. The section includes ultraviolet-visible spectroscopy, fluorescence, infrared and Raman spectroscopy, and X-ray spectrometry. Detection limits are listed for the elements when using flame emission, flame atomic absorption, electrothermal atomic absorption, argon induction coupled plasma, and flame atomic fluorescence. Nuclear magnetic resonance embraces tables for the nuclear properties of the elements, proton chemical shifts and coupling constants, and similar material for carbon-13, boron-11, nitrogen-15, fluorine-19, silicon-19, and phosphoms-31. 

For inductively coupled plasma atomic emission spectroscopy (ICP-AES) the sample is normally in solution but may be a fine particulate solid or even a gas. If it is a solution, this is nebulized, resulting in a fine spray or aerosol, in flowing argon gas. The aerosol is introduced into a plasma torch, illustrated in Figure 3.21. 

A wider range of elements is covered by ICT-AES than by atomic absorption spectroscopy. All elements, except argon, can be determined with an inductively coupled plasma, but there are some difficulties associated with He, Ne, Kr, Xe, F, Cl, Br, O and N. 

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