Instrumental neutron activation analysis as a tool for assessing the solubility of soil mineral matter in strong acid

Fifty samples of natural surface soils with high but variable organic matter content were analyzed for 13 elements (Na, Al, K, Sc, V, Cr, Mn, Fe, Co, Zn, Sr, Ba, La) by INAA. The same samples were analyzed for the “total-recoverable” fraction of these elements by ICP-OES after decomposition with 7M HNO₃, and the results are compared. The data are discussed separately for two groups of samples with organic matter contents of respectively >80% and <70%. In the group with < 70 % organic matter the “total-recoverable” fractions show the following sequence (% of total): Co (83)>Mn (77)>La (60)>Fe=Zn (53)>V (33)>Cr (29)>Sc (25)>Al=Ba (17)>Sr (13)>K (5)>Na (2). The results are in good agreement with corresponding literature data for mineral soils in the case of Al, K, Sc, V, Cr, Fe, and La. In the case of Na, Mn, Co, Zn, Sr, and Ba the present surface soils showed significantly higher “total-recoverable” fractions than the previously studied subsoils. Possible reasons for these differences are discussed. INAA remains a convenient reference technique for determination of total concentrations with the rapidly increasing use of strong mineral acids in environmental studies of elements. This revised version was published online in July 2006 with corrections to the Cover Date.     

Extraction-chromatographic system TBP-HBr in radiochemical neutron activation analysis of high-purity materials

The extraction and extraction-chromatographic behaviour of a variety of elements in the TBP-HBr system with concentrations from 0.1 to 7M HBr has been studied. The results allowed the development of simple procedures for radiochemical neutron activation determination of 22 impurity elements (Na, K, Sc, Cr, Mn, Fe, Co, Ni, Cu, Ga, As, Se, Rb, Sr, Zn, Mo, Ag, Sb, Te, Ba, La, Hf and W) in high-purity cadmium and indium samples with detection limits from 1 g g^–1 for Fe and Zr to 0.01 ng g^–1 for Na, Sc, Mn with relative standard deviations < 0.15. To increase the selectivity of the extraction-chromatographic separation, use was made of extraction suppression and co-extraction effects. The procedure for the extraction-chromatographic separation of scandium from a number of other elements is described as an example. The procedure can be used for simultaneous quantitative separation of impurity radionuclides from radiation produced long-life scandium radionuclides in the neutron activation analysis of titanium and vanadium.     

Trace Elements in Pleurotus Ostreatus,P. Eryngii,and P. Nebrodensis Mushrooms Cultivated on Various Agricultural By-Products

Abstract

Mushrooms are efficient accumulators of essential and toxic elements. Although oyster (Pleurotus spp.) mushrooms are widely commercialized and consumed, few data exist regarding trace elements content and bioaccumulation in cultivated P. ostreatus and P. eryngii, while no data are available for P. nebrodensis. The contents of Al, As, Ba, Cd, Co, Cr, Cs, Cu, Fe, K, Mn, Na, Ni, Pb, Rb, Sr, V, and Zn were monitored using inductively coupled plasma-mass spectrometry (ICP-MS) and atomic emission spectrometry (AES) in P. ostreatus, P. eryngii, and P. nebrodensis mushrooms and their cultivation substrates that include wheat straw (WHS), grape marc (GMC), olive leaves (OLV), and two-phase olive mill wastes (OMW), separately or in mixtures. Bioaccumulation factors (BAFs) less than 0.3 were obtained for Al, Ba, Co, Cr, Fe, Mn, Ni, Pb, Sr, and V; BAFs exceeding 1 for K?>?Zn?>?Cd?>?Cr?>?Rb?>?As, while the BAFs for Na were less 0.7. Mushrooms grown on OLV and OMW presented lower BAFs than those grown on WHS and GMC for all elements except for K, Cd, and Cu. P. ostreatus was an effective accumulator for Cr, Fe, and Zn; P. eryngii for Al, Cs, Ni, and V; and P. nebrodensis for As and Cd. The estimated daily intakes (μg kg^?1 body weight) from mushroom consumption were less than 0.010 for As, Cd, Co, Cs, Pb, and V, 0.010–0.10 for Ba, Cr, Ni, and Sr, 0.10–5.0 for Al, Cu, Fe, Mn, Rb, and Zn, 65–83 for Na, and 858–1030 for K. Overall, the mushrooms studied provide significant amounts of K, adequate amounts of Mn and Zn and low amounts of Na and toxic elements.     

Radiochemical multielement neutron activation analysis of niobium via medium- and long-lived radionuclides

Two radiochemical neutron activation analysis techniques capable for the determination of Ag, Au, Cd, Co, Cr, Cs, Cu, Fe, Hf, Ir, K, Mn, Mo, Na, Ni, Pd, Pt, Rb, Sc, Se, Ta, Th, Sn, W, Zn, and Zr in niobium via medium- and long-lived indicator radionuclides were developed. They involve two different irradiation and cooling times as well as two different group separation schemes based on extraction and ion exchange. The achievable limits of detection are between 10⁻⁷ g/g and 10⁻¹³ g/g. The techniques were applied to analysis of niobium of different purity grades. For a number of elements, the results of these techniques are compared with those of other techniques. This work was supported by Bundesministerium für Forschung und Technologie, Bonn.     

A comparative study of trace elements in water from various sources in surrounding areas of Nagpur city (India) by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) has been used for the determination of 27 elements (Ag, Au, Ba, Br, Ce, Co, Cr, Cs, Eu, Fe, Ga, Hg, Hf, K, La, Mn, Na, Sb, Sc, Se Sr, Th, P, Ta, Tb, Zn and Zr) in 15 water samples collected from different sources (reservoirs, well, borewell, sewage tank, river, rain) in and around Nagpur city (central India) including doubly distilled and a sea water sample from Bombay. Sample residues after evaporation were irradiated at a thermal neutron flux of 10¹²–10¹³ n·cm^–2·s^–1 for 10 min, 1d and 1wk and counted using a HPGe detector and an 4k MCA at different intervals. Several environmental standards from NIST (USA), NIES (Japan) and USGS rock were also analysed for quality assurance. Wide variations in elemental concentrations have been observed in water samples from different sources. Most elemental concentrations in drinking water from various sources, are within ISI/WHO limits. Sea water showed very high concentrations of Ba, Cr, Co, Fe, Hg, Sb, Se and Zn. For doubly distilled and rain waters, however, very low elemental concentrations of Ba, Ce, Fe, Sc, Hg, Se, Sr and Th were observed.     

Determination of 21 elements by INAA for certification of SRM 1570a,Spinach

Analyses for certification have been made by instrumental neutron activation analysis (INAA) for the determination of 21 elements in the National Institute of Standards and Technology (NIST) Spinach renewal reference material, SRM 1570a. Elements determined included ones with short halflife products (Al, V, Ca, Mg), intermediate halflife products (Mn, Na, K, La), and long halflife products (Ba, Co, Cr, Cs, Eu, Fe, Rb, Sb, Sc, Se, Sr, Th, and Zn). For the first time a new robotic sample changer was used in the counting of long halflife indicator isotopes for certification of an SRM. Uncertainties obtained averaged±1.80% for the four major and minor constituents (Ca, K, Mg, Na); ±3.14% for elements with concentrations from 1 to 400 mg/kg (Al, Ba, Cr, Fe, Mn, Rb, Sr, and Zn); and±8.31% for the ultra trace elements (<1 mg/kg) (Co, Cs, Eu, La, Sb, Sc, Se, Th, and V).     

Elemental composition studies of fugitive and ambient air dust particulates from a thermal power station by instrumental neutron activation analysis

In order to assess the source of pollutants and the atmosphere quality in and around a thermal power plant, fugitive dust particulates from seven different locations and ambient air dust from six locations have been analyzed for 32 elements (As, Au, Ba, Br, Ce, Cl, Co, Cr, Cs, Cu, Eu, Fe, Ga, Hg, Hf, K, La, Lu, Mg, Mn, Na, P, Rb, Sb, Sc, Se, Ta, Tb, Te, Th, W and Yb) by employing instrumental neutron activation analysis (INAA). The method involves the irradiation of samples and comparator standards in a thermal neutron flux range of 10¹²–10¹³ n·cm^–2·s^–1 in a nuclear reactor for 10 min and 1 day followed by high resolution -spectrometry. Wide differences have been observed in the mean elemental concentrations of Fe, Co, Br, Mn, As, P. Ba and Cu in fugitive and ambient dust particulates coliected from these different locations. Further, a comparison of the elemental contents of the dust particulates from the plant with environmental standards (Urban Particulate Matter, Coal Fly Ash, Vehicle Exhaust and Coal) show significantly lower or comparable amounts of toxic and pollutant elements in the environmental samples.     

Determination of uranium, thorium, and 20 other elements in high-purity tungsten by radiochemical neutron activation analysis

A radiochemical neutron activation analysis method for the determination of 22 elements in high-purity tungsten has been developed. For the assay of indicator radionuclides with long half-lives, the radiochemical separation was performed from HF/H₂O₂, HF/NH₄F and HCl/H₂SO₄ media by a combination of cation and anion exchange on a Dowex 50 W × 8 and Dowex 1 × 8 column. An effective removal of the matrix-produced radionuclides of W and Re was achieved. U was determined via ¹⁴⁰La, the daughter nuclide of the fission product ¹⁴⁰Ba. Limits of detection of 2 ng/g for U and 0.02 ng/g for Th can be achieved. For the other elements, the limits of detection are between 0.004 ng/g (Sc) and 200 ng/g (Sr). The elements Hf, Ta and Sb could be determined by instrumental neutron activation analysis. This method was applied to the analysis of two tungsten powder samples of different purity grade. The results and limits of detection are compared with those of other methods.     

Determination of U,Th and other impurities in molybdenum by radiochemical neutron activation analysis

A radiochemical separation method has been applied for determining uranium, thorium and other impurities in molybdenum metallic powder. The impurities of Na, K, Sm, Cr, Zr, Cs, Rb, Zn, Fe, Co and La were separated with a cation exchange resin, and uranium and thorium were, then, separated with an anion exchange resin. The content of impurities were determined by a single comparator method using two monitors, gold and cobalt.     

Assessing sediment pollution from the Julian Adame-Alatorre dam by instrumental neutron activation analysis

The rapid industrial development in regions of Mexico during recent years has had the side effect of introducing toxic metals, fertilizers, and pesticides into the ecosystem. Sediment cores were collected from eight locations around the Julian Adame-Alatorre dam located in the Municipality of Villanueva in the State of Zacatecas, México. The cores were analyzed for 32 major, trace, and rare earth elements (As, La, Lu, Nd, Sm, U, Yb, Ce, Co, Cr, Cs, Eu, Fe, Hf, Rb, Sb, Sc, Sr, Ta, Tb, Th, Zn, Zr, Al, Ba, Ca, Dy, K, Mn, Na, Ti, and V) in order to estimate the health risk. The samples were analyzed by instrument neutron activation analysis (INAA) using thermal neutron fluxes of 8 × 10¹³ and 5 × 10¹³ n cm⁻² s⁻¹ for short and long irradiations, respectively. The results of the contamination levels for elements such as As, Ba, Cr, Fe, Mn, Ta, V, and Zn were compared with the Mexican regulations and the guidelines of USEPA. Enrichment factors for quantified elements identified high As, Sb, Hf, and Cs contents using Fe as a crustal reference.     

Preparation of <Superscript>26</Superscript>Al, <Superscript>59</Superscript>Ni, <Superscript>44</Superscript>Ti, <Superscript>53</Superscript>Mn and <Superscript>60</Superscript>Fe from a proton irradiated copper beam dump

The station for pions cancer therapy was operated at PSI from 1980 to 1992. After a cooling time of 12 years it’s made of copper beam dump was cut and samples were taken for analytical purposes. The sampling collected about 500 g of high active copper chips that can be used for separation of exotic radionuclides. The analyses by gamma spectrometry, LSC and AMS showed main nuclides present to be ⁶⁰Co, ⁵⁴Mn, ²²Na, ⁶⁵Zn, ²⁶Al, ⁵³Mn, ⁵⁹Ni, ⁶³Ni, ⁵⁵Fe and ⁶⁰Fe and ⁴⁴Ti with a daughter nuclide ⁴⁴Sc. In the frame of ERAWAST project a procedure combining selective precipitation and ion exchange for the separation of the rare radionuclides from the copper beam dump was developed. The proposed separation procedure is easy for remote controlled implementation in a hot cell. The ion exchange separation of Ni, Al, Mg, Ti and Fe was complete and high decontamination factors for copper and cobalt were achieved. Based on the developed procedure a remotely controlled system for separation of exotic radionuclides from the copper chips was set up. The full scale system was installed in a hot cell where high activity levels can be handled. In order to evaluate the reliability and functionality of the system extensive tests have been done. During the test period 13.86 g in total of the proton irradiated copper beam dump were processed for separation of ²⁶Al, ⁵⁹Ni, ⁵³Mn, ⁴⁴Ti and ⁶⁰Fe. The results showed that the system was operational and the radionuclide separation was selective with high chemical yield. The procedure manages as well the generated liquid wastes containing high level of ⁶⁰Co activity.     

Elemental analysis of brahmi (<Emphasis Type="Italic">Bacopa</Emphasis> <Emphasis Type="Italic">monnieri</Emphasis>) extracts by neutron activation and its bioassay for antioxidant,radio protective and anti-lipid peroxidation activity

Brahmi (Bacopa monnieri) leaves, known as nervine tonic in Ayurveda, and its aqueous (BA), methanolic (BM) and aqueous–methanolic (BAM) extracts were analyzed for 7 minor (Al, Fe, Na, K, Ca, P, Cl) and 18 trace (As, Au, Ba, Br, Co, Cr, Cu, Hf, Hg, La, Mn, Rb, Se, Sm, Sr, Th, V, Zn) elements by INAA. BAM extract showed maximum contents of Na, K, Cl and significant amounts of Mn, Co, Zn. It was also found as effective scavenger of DPPH radicals with 33.5% total phenolic content, highest γ-ray radioprotective effect and higher anti lipid peroxidation activity.     

Determination of uranium, thorium, and 20 other elements in high-purity tungsten by radiochemical neutron activation analysis

A radiochemical neutron activation analysis method for the determination of 22 elements in high-purity tungsten has been developed. For the assay of indicator radionuclides with long half-lives, the radiochemical separation was performed from HF/H₂O₂, HF/NH₄F and HCl/H₂SO₄ media by a combination of cation and anion exchange on a Dowex 50 W × 8 and Dowex 1 × 8 column. An effective removal of the matrix-produced radionuclides of W and Re was achieved. U was determined via ¹⁴⁰La, the daughter nuclide of the fission product ¹⁴⁰Ba. Limits of detection of 2 ng/g for U and 0.02 ng/g for Th can be achieved. For the other elements, the limits of detection are between 0.004 ng/g (Sc) and 200 ng/g (Sr). The elements Hf, Ta and Sb could be determined by instrumental neutron activation analysis. This method was applied to the analysis of two tungsten powder samples of different purity grade. The results and limits of detection are compared with those of other methods. Received: 28 July 1997 / Revised: 29 October 1997 / Accepted: 1 November 1997     

Evaluation of strontium isotope abundance ratios in combination with multi-elemental analysis as a possible tool to study the geographical origin of ciders

In order to evaluate alternative analytical methodologies to study the geographical origin of ciders, both multi-elemental analysis and Sr isotope abundance ratios in combination with multivariate statistical analysis were estimated in 67 samples from England, Switzerland, France and two Spanish regions (Asturias and the Basque Country). A methodology for the precise and accurate determination of the ⁸⁷Sr/⁸⁶Sr isotope abundance ratio in ciders by multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) was developed. Major elements (Na, K, Ca and Mg) were measured by ICP-AES and minor and trace elements (Li, Be, B, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Cd, Sn, Sb, Cs, Ba, La, Ce, W, Tl, Pb, Bi, Th and U) were measured by ICP-MS using a collision cell instrument operated in multitune mode. An analysis of variance (ANOVA test) indicated that group means for B, Cr, Fe, Ni, Cu, Se, Cd, Cs, Ce, W, Pb, Bi and U did not show any significant differences at the 95% confidence level, so these elements were rejected for further statistical analysis. Another group of elements (Li, Be, Sc, Co, Ga, Y, Sn, Sb, La, Tl, Th) was removed from the data set because concentrations were close to the limits of detection for many samples. Therefore, the remaining elements (Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba) together with ⁸⁷Sr/⁸⁶Sr isotope abundance ratio were considered for principal component analysis (PCA) and linear discriminant analysis (LDA). Finally, LDA was able to classify correctly 100% of cider samples coming from different Spanish regions, France, England and Switzerland when considering Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba and ⁸⁷Sr/⁸⁶Sr isotope abundance ratio as original variables.     

Computer assisted multielement analysis of terrestrial and extraterrestrial materials and studies on long-lived cosmogenic53Mn by neutron activation

In a large number of alpine rocks and respective mineral separates the beryllium distribution was studied via “non-destructive” photon activation. The detection limit of the assembly was ∼20 ppb. The existence of Be-rich areas was revealed. A selection of individual rocks was analysed by instrumental as well as by radiochemical neutron activation analysis for main and trace elements as: Na, K, Sc, Cr, Mn, Fe, Co, Rb, Cs, La, Eu, Yb, Ta, W, Au, and U. The latter was determined by counting the²³⁵U-fission tracks. The data supply an insight into the complex processes leading to the formation of metamorphic rocks. The hardware and the computer evaluation of the γ-spectra is described in some detail. A further application is the determination of traces of⁵³Mn (in the order of 10⁻¹² g/g) produced by the interaction of cosmic rays with stony meteorites. From a comparison of the²⁶Al- and⁵³Mn-values it is concluded that the depth dependent production of these two radionuclides differs slightly.     

Determination of minor, trace and toxic elements in chewing tobacco products by instrumental neutron activation analysis and identification of glutamic acid

Tobacco smoking/chewing has been a cause of concern because of it being related with oral cancer. It causes stimulation and ill physiological effects. Ten different brands of spit tobacco, eight gutkaas and five paan masalas have been analyzed for seven minor (Al, Na, K, Ca, Cl, Mg, and P) and 17 trace (As, Ba, Br, Co, Cr, Cs, Cu, Eu, Fe, Hg, La, Mn, Rb, Sb, Sc, Th, and Zn) elements by instrumental neutron activation analysis. Also Ni and Pb were determined by atomic absorption spectrophotometry. Concentration of Cd was below detection limit (<10?mg?kg^?1) in the tobacco samples. Mg, generally added as MgCO₃ to prevent caking, is present as minor constituent in spit tobacco and gutkaas but is below detection limit (<1?g?kg^?1) in paan masalas. Most elemental concentrations vary in a wide range depending on the nature of chewing tobacco. Spit tobacco has been found to be more enriched in essential elements (Ca, K, Na, P, Mn, and Rb), whereas gutkaas contain higher concentrations of Fe, Cr, Cu, and Zn. Paan masalas contain lower contents of other elements but higher content of Hg. Gutkaas also contain higher amounts of As and Pb. Further glutamic acid has been separated from tobacco leaves and characterized as it might bind with some elements.     

Multielement analysis of green coffee and its possible use for the determination of origin

Using instrumental neutron activation analysis (INAA), graphite furnace atomic absorption spectrometry (GFAAS), flame atomic absorption spectrometry (FAAS) and combustion elemental analysis, green coffees of the Arabica species produced in crop year 1987/88 in Colombia, Costa Rica, Cuba, El Salvador, Mexico, Nicaragua, Panamá and Papua New Guinea were analysed for the elements Ba, Br, C, Ca, Co, Cr, Cu, Cs, Fe, H, K, La, Mg, Mn, N, Na, Rb, Sc, Sr and Zn. In accordance with the concentrations determined, the elements could be ranked into five groups: Sc (sub-ppb level); Br, Co, Cr, Cs and La (ppb level); Ba, Cu, Fe, Mn, Na, Rb, Sr and Zn (ppm level); Ca and Mg (%o level); and C, H, K and N (% level). On the basis of the results obtained, an attempt was made to establish the origin of the green coffee via its elemental composition. Among the investigated elements, manganese was found to be best suited as an indicator for this purpose. However, the elements C, Co, Cs, Na and Rb proved to be of interest too.     

Assessment of metal contamination in an urban drainage system (using water and tilapia, Oreochromis spp.) in view of human health effect. A case study of some selected communities in Cape Coast township in Ghana

This research work aimed at studying the metal content of water and tilapia fish sample, Oreochromis spp., from a wastewater-fed pond around the University of Cape Coast community using instrumental neutron activation analysis. The metals studied were Al, As, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, V and Zn. In the water samples the order of elemental concentrations at sampling point 1, in ??g/g, was K (75.96?±?0.92), Na (18.52?±?0.35), Al (6.00?±?0.89), Mn (3.28?±?0.44), As (3.08?±?0.40), Mg (1.56?±?0.17), Ca (0.70?±?0.08), Cu (0.54?±?0.08) and V (0.04?±?0.01). Co, Cr, Fe and Zn were below detection limits of INAA. The order of elemental concentrations in the water at point 2 was as follows: Na (4.99?±?0.14), K (4.82?±?0.89), Mn (4.40?±?0.53), Mg (2.92?±?0.37), Al (1.98?±?0.21), As (0.69?±?0.10), Ca (0.24?±?0.07) and V (0.23?±?0.06) with Co, Cr, Cu, Fe and Zn falling below the detection limit of INAA. The concentrations recorded for Al, As, Cu and Mn in the water samples were all above WHO permissible limits. The mean levels of heavy metals in the soft tissue of tilapia was of the order: K?>?Mg?>?Fe?>?Ca?>?Na?>?Al?>?Mn?>?Zn?>?V?>?Cu?>?Cr?>?Co. Arsenic was below detection limit. The transfer factor values calculated for the metals Al, Ca, K, Mg, Mn, Na and V were all greater than one indicating movement of metals from the water column to the tilapia species. The hazard index (HI) calculated for Al, Fe, Mn and V suggested possible occurrence of adverse health effects (HI?>?1) where as the HI value obtained for Cr, Cu and Zn (i.e., HI?<?1) suggested unlikely adverse effects occurring.     

Determination of 32 elements in rocks by neutron activation analysis and high resolution gamma-ray spectroscopy

Neutron activation analysis and Ge(Li) spectroscopy was used to determine 32 elements in seven U.S.G.S. standard rocks of a wide range of composition. Short half-life nuclides (10 sec-10 min) were used to measure Sc, Hf, Dy, Mg, Al, Ca, Ti, V (and Na) in an automated rabbit Ge(Li) detector system. The elements K, Cu, Zn, Ga, Sr, Ba, La, Eu, Sm (and Mn) were determined by dissolution of the irradiated sample followed by removal of²⁴Na on hydrated antimony pentoxide (HAP). Long-lived nuclides were used to measure Sc, Cr, Fe, Co, Zr, Rb, Sb, Cs, Ba, Ce, Eu, Yb, Tb, Lu, Hf, Ta and Th after decay of²⁴Na. The method involves little radiochemistry and the separation is selective for²⁴Na under the experimental conditions used. Elemental concentrations determined agree well with previously published data.     

Heavy elements concentrations,physiochemical characteristics and natural radionuclides levels along the Saudi coastline of the Gulf of Aqaba

This paper represents the first work on the concentrations of heavy elements, physiochemical characteristics and activity levels of the naturally occurring radionuclides in the Saudi Arabian coastline of the Gulf of Aqaba. Concentrations of 19 heavy elements were measured, namely: Ag, Al, As, Ba, Be, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Sb, Se, V and Zn. The radioactivity levels of ²³⁸U, ²³²Th and ⁴⁰K were estimated to be: 17 ± 1.7, 22.5 ± 3.7 and 649.6 ± 64.2 Bq kg^?1, respectively. The measurements were carried out using inductively coupled plasma-mass spectrometry (ICP-MS). In addition, physiochemical characteristics of 19 sediment samples (i.e., saturation percentage, pH, electrical conductivity, organic matter, cation exchange capacity and content of clay, silt and sand) have been determined. Indications for high correlation between most heavy elements are found. The correlation between heavy elements and the radionuclides ²³⁸U, ²³²Th and ⁴⁰K was generally significant.