Environmental Instrumental Activation Analysis

Kucera J, and Soukal L (1998) Low uncertainty determination of manganese and vanadium in environmental and biological reference materials by instrumental neutron activation analysis. Fresenius J Anal Chem 360 415-418. 

Salmon, L., Instrumental Neutron Activation Analysis in Environmental Studies of Trace Elements, AERE-R 7859, HMSO, 1975. 

WVGES has not had analytical laboratory facilities since the 1970 s so contract geochemical analyses are a necessity. After considering a variety of sources for analytical work including both university and government laboratories, we decided to use a commercial lab, located in Ontario, which specializes in analyses for the mineral exploration industry (they have since expanded into the environmental field as well). For the sake of consistency, each sample is analyzed using the same set of techniques, a combination of Instrumental Neutron Activation Analysis (INAA) and Selective Extraction-Ignition Coupled Plasma spectroscopy that yield results for 49 elements - Au, Ag, As, Ba, Br, Ca, Co, Cr, Cs, Fe, Hf, Hg, Ir, Mo, Na, Ni, Rb, Sb, Sc, Se, Sn, Sr, Ta, Th, U, W, Zn, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu, Cu, Pb, Mn, Cd,... 

With analytical methods such as x-ray fluorescence (XRF), proton-induced x-ray emission (PIXE), and instrumental neutron activation analysis (INAA), many metals can be simultaneously analyzed without destroying the sample matrix. Of these, XRF and PEXE have good sensitivity and are frequently used to analyze nickel in environmental samples containing low levels of nickel such as rain, snow, and air (Hansson et al. 1988 Landsberger et al. 1983 Schroeder et al. 1987 Wiersema et al. 1984). The Texas Air Control Board, which uses XRF in its network of air monitors, reported a mean minimum detectable value of 6 ng nickel/m (Wiersema et al. 1984). A detection limit of 30 ng/L was obtained using PIXE with a nonselective preconcentration step (Hansson et al. 1988). In these techniques, the sample (e.g., air particulates collected on a filter) is irradiated with a source of x-ray photons or protons. The excited atoms emit their own characteristic energy spectrum, which is detected with an x-ray detector and multichannel analyzer. INAA and neutron activation analysis (NAA) with prior nickel separation and concentration have poor sensitivity and are rarely used (Schroeder et al. 1987 Stoeppler 1984). 

Increased environmental concern has accelerated research on the analysis of trace elements in fuels in many university and governmental facilities. Because instruments such as mass spectrometers and nuclear reactors for neutron activation analysis are available, much of this research uses sophisticated instrumentation and techniques. However, the wet chemistry laboratory is still the only available source of chemical... 

Methods and technology were developed and used at the NASA Plum Brook Reactor (PBR) to analyze trace elements in pollution-related samples by instrumental neutron activation analysis (INAA). This work is significant because it demonstrates that INAA is a useful analytic tool for monitoring trace elements in a variety of sample matrices related to environmental protection. In addition to coal, other samples analyzed for trace elements included fly ash, bottom ash, crude oil, fuel oil, residual oil, gasoline, jet fuel, kerosene, filtered air particulates, various ores, stack... 

Battelle has developed instrumental neutron activation analysis (INAA) techniques which permit very sensitive and accurate multielement analysis of approximately 40 elements in coal and fly ash. These techniques, which will be described in this work, form the basis for extensive environmental studies of the effluent from coal-powered generating facilities and other pollution sources. 

Detection techniques of high sensitivity, selectivity, and ease of coupling with sample preparation procedures are of special interest for measuring PGM content in biological and environmental samples. ICP MS, electrothermal atomic absorption spectrometry (ET AAS), adsorptive voltammetry (AV), and neutron activation analysis (NAA) have fotmd the widest applications, both for direct determination of the total metal content in the examined samples and for coupling with instrumental separation techniques. Mass spectrometry coupled with techniques such as electrospray ionization (ESI) and capillary electrophoresis (CE) (e.g., ESI MS", LC ESI MS", LC ICP MS, CE MS", and CE ICP MS) offer powerful potential for speciation analysis of metals. MS is widely used for examination of the distribution of the metals in various materials (elemental analysis) and for elucidation of the... 

Heft, R.E. Absolute Instrumental neutron-activation analysis at Lawrence Livermore Laboratory Third Intern Conf. on Nuclear Methods in Environmental and Energy Research, October 10-13, 1977. 

Suzuki S, Hirai S. 1987. Instrumental neutron activation analysis of vehicle exhaust particulates as environmental reference material. Anal Sci 3 193-197. 

X-ray fluorescence spectrometry (XRF) and instrumental neutron activation analysis (INAA) are commonly used for multi-element analysis of rock, soil, and sediment samples since they do not require chemical dissolution. However, the detection limit for arsenic using XRF is on the order of 5 mg kg and is too high for many environmental purposes. Once dissolved, arsenic can be determined using many of the methods described above... 

In instrument neutron activation analysis (INAA) a small fraction of the stable atomic nuclei present in the sample are made radioactive by irradiation with neutrons or other particles. By measuring the resulting radioactivity, the original elements present can be determined. Reactor or thermal neutrons are usually used. The method does not work well for certain key elements of environmental interest including silicon, sulfur, and lead. Table 6.2 shows INAA detection limits for various elements and typical concentrations of these elemenis in urban air. In atmospheric samples, the fiiiiii of detectability for a particular clement depends on the quantities of the other elements in the filter matrix. The table is based on a total air sample of 17 actually used in the measurements. The tabulated results show that all elements listed could be detected in this air volume with the exception... 

NAA has been used to determine selenium levels in environmental samples. Dams et al. (1970) reported a detection limit of lxlO 10 g/m3 selenium using nondestructive NAA for determining selenium in air particulate matter. For determining selenium levels in soil, radiochemical variants of NAA have been commonly employed (Bern 1981). Instrumental neutron activation analysis (INAA) is frequently used to determine selenium concentrations in water and can also be used to distinguish between selenium(IV) and selenium(VI) oxidation states (Bern 1981). INAA is also used to determine selenium concentrations in air (Bern 1981). 

Gether, J., G. Lunde, and E. Steinnes. 1979. Determination of the total amount of organically bound chlorine, bromine and iodine in environmental samples by instrumental neutron activation analysis. Anal. Chim. Acta 108 137-147. 

In the course of determinations of trace element concentrations in nails of a group of carpenters by cyclic instrumental neutron activation analysis (CINAA) using the PCA (principal component analysis256-259) method, the silver concentration in nails was determined260 to be 0.027 0.037 pgg-1. The mean concentration of gold was 0.010 pgg-1. Nails can be used as a dietary and environmental exposure monitor261-267. 

Some examples of applications of nuclear activation analytical techniques to elemental determinations in a variety of materials are presented in Table 2.10. The specific contents of some of these and other publications may be briefly highlighted. Cunningham and Stroube Jr. (1987) provide a nice coverage of the application of an instrumental neutron activation analysis procedure to analysis of food, describing the capabilities of INAA for the multielement analysis of foods as carried out for many years, and also currently, by analysts of the US Food and Drug Administration stationed at the NIST Nuclear reactor facility. Salbu and Steinnes (1992) touch upon applications of nuclear analytical techniques in environmental research, and Norman and Iyengar... 

Filby, R.H., Davis, A.I., Shah, K.R. and Haller, W.A. (1970) Determination of mercury in biological and environmental materials by instrumental neutron activation analysis. Microchim. Acta, 1970, 1130-1136. 

Bode, P., Wolterbeek, Fl.Th., 1990. Environmental research and instrumental neutron activation analysis aspects of high accuracy and multi-element capability. J. Trace Microprobe Technol. 8, 121-138. 

In order to evaluate possible hazards for the enviroiunent and human health it is crucial to develop analytical strategies for fast and easy quantification of traces and ultra-traces of Pd in environmental matrices as well as biological tissues and fluids. Despite the efforts of numerous workgroups, a reliable method for the determination of Pd in all environmental matrices has yet to be developed. Up to date, the most important analytical methods for this task are electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma-mass spectrometry (ICP-MS) and isotope dilution (ID)-ICP-MS, also strategies involving inductively coupled plasma-atomic emission spectrometry (ICP-AES), and electrochemical methods like anodic stripping voltammetry (ASV) have been described. Furthermore, total reflection X-ray fluorescence (TXRF) and instrumental neutron activation analysis (INAA) have been successfully employed for the determination of PGE in enviromnental matrices. 

Neutron activation analysis is one of the major techniques for the determination of many minor and trace elements in a large variety of solid environmental and pollution samples, such as atmospheric aerosols, particulate emissions, fly ash, coal, incineration ash, and sewage sludge. Instrumental neutron activation analysis of total, inhal-able, or respirable airborne particulate matter collected on a cellulose or membrane filter, or in a cascade impactor on some organic substrate, allows the determination of up to 45 elements by an irradiation - counting scheme similar to the one given in Figure 3. Radiochemical NAA is applied only when extremely low limits of determination are required. Instrumental photon activation analysis is also complementary to INAA. 

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