Determination of uranium fission interference factors for INAA

Instrumental neutron activation analysis (INAA) is a very suitable technique for the determination of several elements in different kinds of matrices. However, when the sample contains high uranium concentration this method presents interference problems of uranium fission products. The same radioisotopes used in INAA are formed in uranium fission. Among these radioisotopes are ¹⁴¹Ce, ¹⁴³Ce, ¹⁴⁰La, ⁹⁹Mo, ¹⁴⁷Nd, ¹⁵³Sm and ⁹⁵Zr. The purpose of this study was to evaluate uranium fission interference factors to be used in the INAA of environmental and geological samples containing high levels of U. The obtained interference factors agreed with literature reported values. The results point to the viability of using these experimentally determined interference factors for the correction of uranium fission products.     

Comparison of instrumental neutron activation analysis of geological materials with other multielement techniques

Results obtained for 12 elements in approximately 1600 rocks by instrumental neutron activation analysis (INAA) are compared with those obtained by ICP emission spectrometry (ICP-ES), XRF, and atomic-absorption spectrometry (AAS). Sample duplicates and two controls are used to evaluate the precison of the methods investigated. Application of a method (Maximum Likelihood Functional Relationship) to determine and quantify rotational and translational bias is demonstrated. The elements Na, Fe, Ba, Co, Cr, La, Ni and Rb can be determined in rocks by INAA with sufficient sensitivity and precision, whereas the determination of Ag, Yb, Zn and Zr suffers from inadequate sensitivity. Good agreement is seen in the results for Na (by INAA, ICP-ES and XRF) and AG (INAA and AAS). A significant positive bias (13% or less) is evident in the comparison of results by INAA and ICP-ES or XRF for Cr, Ba, Ni and Fe over a wide range of concentration. A similar trend, though less significant, is observed for the elements Yb, Rb, La and Co; the upper limit of concentration for satisfactory determination is within a decade of the highest detection limit for these elements. Rotational and translational bias is evident for Zn in the comparison of data obtained by INAA and ICP-ES, the results by INAA being appreciably lower above about 400 ppm Zn.     

Determination of traces of elemental impurities in single walled (SWNT) and multi walled (MWNT) pristine and purified carbon nanotubes by instrumental neutron activation analysis

By using instrumental neutron activation analysis (INAA) it has been shown that some pristine carbon SWNT's and MWNT's of different makes, contain a multitude of trace element impurities at various concentration levels including also amounts which can be considered as nanoelectronically dopant quantities. The same holds for the above mentioned carbon nanotubes also after their inadequately so-called purification. This revised version was published online in July 2006 with corrections to the Cover Date.     

Elemental contents in hair of children from Zanzibar in Tanzania as bio-indicator of their nutritional status

Nutritional status and toxic elements body burden were evaluated in hair of children living in Zanzibar. 18 samples were collected from Zanzibar town and 19 samples from Nungwi village, which is approximately 64 km from Zanzibar town. The analysis was carried out using instrumental neutron activation analysis (INAA). The concentration ranges obtained in this study overlap with the published elemental values of healthy children of the same age group. The concentration levels of K, Zn, Cu, As and Co in hair of children from Zanzibar town were higher than from Nungwi whereas levels of Mn, Br and Sr were lower.     

Application of INAA and XRFA in a comparative environmental study

Environmental monitoring requires reliable and effective analytical techniques for widely different concentration ranges. Two such methods (INAA and XRFA) were applied in a comparative environmental study on air dust filters and grass. The samples were collected during one year at two locations (near Bucharest/Romania and near Stuttgart/Germany) with different levels of air pollution. Seventeen environmentally relevant elements (As, Ba, Br, Ca, Co, Cr, Cu, Fe, K, Mn, Ni, Pb, S, Sb, Se, V, Zn) were determined. The aim was to test the suitability of INAA and XRFA methods for different elements in these kinds of samplesaat realistical pollution levels. The results were statistically compared for 13 elements, which were determined by both analytical techniques. They were also used to characterize the air pollution level and its variation at the two locations, and to compare them. Generally, concentrations in air of the elements studied are higher in Bucharest than in Stuttgart.     

INAA and ETAAS of toxic element content of fruits harvested and consumed in Pakistan

Instrumental neutron activation analysis (INAA) and electro-thermal atomic absorption spectrometry (ETAAS) were employed to determine the toxic elements in fourteen fruits harvested in Pakistan. As, Br, Hg, Sb and Se were determined using INAA. Cadmium and Pb were determined using ETAAS. The intake levels of all toxic elements have been calculated. The data show that dates supply the maximum amount of most of the toxic elements. Peels of apple and pear have also been investigated and were found to contain higher concentration of toxic elements than their edible parts. The reliability of the techniques has been established by the use of standard reference materials. This study shows that all investigated fruits cultivated and consumed in Pakistan are safe for human consumption.     

Use of combined NAA and SIMS analyses for impurity level isotope detection

Instrumental neutron activation analysis (INAA) and electro-thermal atomic absorption spectrometry (ETAAS) were employed to determine the toxic elements in fourteen fruits harvested in Pakistan. As, Br, Hg, Sb and Se were determined using INAA. Cadmium and Pb were determined using ETAAS. The intake levels of all toxic elements have been calculated. The data show that dates supply the maximum amount of most of the toxic elements. Peels of apple and pear have also been investigated and were found to contain higher concentration of toxic elements than their edible parts. The reliability of the techniques has been established by the use of standard reference materials. This study shows that all investigated fruits cultivated and consumed in Pakistan are safe for human consumption.     

Investigate the capability of INAA absolute method to determine the concentrations of 238U and 232Th in rock samples

This work aimed to study the capability of INAA absolute method in determining the elemental concentration of ²³⁸U and ²³²Th in the rock samples. The INAA absolute method was implemented in PUSPATI TRIGA Mark II research reactor, Malaysian Nuclear Agency (NM). The accuracy of INAA absolute method was performed by analyzing the IAEA certified reference material (CRM) Soil-7. The analytical results showed the deviations between experimental and certified values were mostly less than 10 % with Z-score in most cases less than 1. In general, the results of analysed CRM Soil-7 show a good agreement between certified and experimental results which mean that the INAA absolute method can be used accurately for elemental analysis of uranium and thorium in various types of samples. The concentration of ²³⁸U and ²³²Th ranged from 1.77 to 24.25 and 0.88 to 95.50 ppm respectively. The highest value of ²³⁸U and ²³²Th was recorded for granite rock sample G17 of ²³⁸U and sample G9 of ²³²Th, whereas the lower value was 1.77 ppm of ²³⁸U recorded in sandstone rock and 0.88 ppm of ²³²Th for gabbro. Moreover, a comparison of the ²³⁸U and ²³²Th results obtained by the INAA absolute method shows an acceptable level of consistency with those obtained by the INAA relative method.     

Mercury and cadmium concentrations in milk in Puerto Rico

Milk was collected over a four-month period from three representative sectors of Puerto Rico. Instrumental neutron activation analysis (INAA) performed on the samples showed that the mercury concentration was slightly higher than the safe upper limit set by the World Health Organisation on food products. INAA for cadmium yielded high values when compared with atomic absorption.     

Nuclear analytical techniques for quantification of uranium for its recovery from seawater

Nuclear analytical techniques namely fission track technique using solid state nuclear track detector (SSNTD) and instrumental neutron activation analysis (INAA) have been standardized and applied for quantification of low uranium concentrations in liquid samples such as feed, elute and brine and solid sorbent samples respectively. The quantification of uranium is required for its recovery study from seawater, which is one of the potential sources of uranium. The uranium concentration of a liquid sample obtained by SSNTD method was compared with the other well established conventional techniques like ICP-MS, ICP-AES, adsorptive stripping voltametry and alpha spectrometry. INAA was applied for uranium concentration determination in the radiation grafted polyamidoxime sorbent samples.     

Multi-element determination in earthworms with instrumental neutron activation analysis and inductively coupled plasma mass spectrometry: A comparison

Earthworms were collected from agricultural fields in Admont, Graz, Piber and Gumpenstein, Austria. Six earthworm samples were investigated with INAA and with ICP-MS in parallel for the element concentrations of As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Pb, Rb, Sb, Se and Zn. With both techniques 14 elements were analysed in a wide concentration range (ng/g to mg/g) GF-AAS and HG-AAS were used for verification of some element concentrations. A comparison of analytical results between INAA and ICP-MS was discussed. In general, good agreement between ICP-MS and INAA was obtained, the relative difference values of most of the elements are within ±20% range, however, a methodical error for the determination of Hg by ICP-MS was found.     

Determination of pollutants in dwellings by neutron activation analysis and X-ray fluorescence

Metallic pollutants were measured in dwellings in Mexico City by instrumental neutron activation analysis (INAA) and X-ray fluorescence techniques. Monitoring was performed in the west side of the city and in the winter season. In general the average concentration of contaminants collected, when compared with the average concentrations reported in a previous paper, have increased with time and in the particular case of lead and mercury some samples are above the indicative WHO maximum levels.     

Minor and Trace Element Determination of Food Spices and Pulses of Different Origins by NAA and PAA

INAA, RNAA and IPAA were employed to determine upto 26 trace elements in 32 spices of 18 species and 16 pulses of 8 species originating from different localities. The results are compared with each other and the reported values. The concentration levels, their variations and the correlations of the analysed elements in these samples were also investigated. The variability of concentrations among the samples of different origin are small. The levels and ranges of the concentration are highly variable which are found to be characteristic to each element. High elemental correlations exist in some sets of elements, reflecting characteristics of chemical nature of elements and/or of their physiological functions.     

Combined application of INAA and PIXE for studying the regional aerosol composition in Southern Africa

As part of the SAFARI-92 biomass buming experiment, aerosol collections were carried out with several size-fractionating sampling devices at a number of sites in Southern Africa. One of the samplers used at all ground-based sites was a stacked filter unit (SFU). The SFU samples were analyzed by both INAA and PIXE analysis. The present paper gives an intercomparison of the analytical results obtained in order to assess the accuracy and to check the quality assurance of the analytical procedures. Twenty-one common elements were determined by both INAA and PIXE. Concentrations of 13 elements (i.e., Na, Mg, Al, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Zn and Br) were generally measured with sufficient precision in both techniques for performing the intercomparison. The INAA and PIXE data were compared in terms of PIXE/INAA concentration ratios on a sample by sample basis for the coarse and fine size fraction separately. the atmospheric concentrations for K, Mn and Fe agreed within 5–10%, the agreement between the data for the other common elements was typically better than 15%. Possible explanations for lower than 1.0 ratios for Cl, Br and Na are presented. The common elements were classified into groups according to their detectability and sensitivity in each technique.     

Instrumental neutron activation analysis to measure short-term accretion and erosion in wetlands using rare earth element soil horizon markers

Instrumental neutron activation analysis (INAA) was employed to estimate sediment accumulations (accretion) in Louisiana in a freshwater wetland habitat four years after the application of rare earth, samarium (Sm) and dysprosium (Dy), soil horizon markers. The sediment cores used to measure accretion also were used to construct a sodium (Na) profile (Na concentration vs. depth) in three locations. Additionally, in a 6-month study INAA data were used to determine the feasibility of using Sm and Dy to estimate the direction and quantity of soil erosion particles in a salt water wetland in Georgia.     

Contamination of crop vegetation with trace elements from a fertilizer plant: An INAA study

Instrumental neutron activation analysis (INAA) was used to determine various trace elements in crop vegetation (potato, carrot and maize) grown around a phosphate fertilizer plant in Romania. INAA using long-lived radionuclides was applied at NIPNE in Bucharest, and based on short-lived radionuclides at JINR in Dubna. The results for Na, Mg, Cl, K, Ca, Mn, Fe, Zn, As, and Hg were compared with Romanian norms for the alimentary products, as well as with literature data. Concentration ratios to control samples for both soil and crop as well as concentration factors of crop to host soil were assessed. This revised version was published online in July 2006 with corrections to the Cover Date.     

Metrology for Chemical Measurements and the Position of INAA

Metrology systems are being established by various countries for the worldwide comparability of data related to trade, industrial products, health, and the environment. This has in turn led to an increased interest in methods that have the highest possible accuracy and precision. The relevance of instrumental neutron activation analysis (INAA) for metrological science has been evaluated. It is concluded that INAA is a suitable technique for method validation, proficiency testing, development of reference materials and reference methods. Moreover, it is concluded that INAA may comply with the CCQM definition of a definitive or primary ratio method provided that the uncertainty in the results is reduced to much lower levels compared to those currently encountered in most NAA laboratories.     

QA/QC Procedures,Validation Method,Traceability and Intercomparisons

Summary This work provides a systematic experimental approach to the demonstration of viability of instrumental neutron activation analysis (INAA) in chemical metrology. The practical approach was derived from a complete survey of uncertainty components that affect the INAA measurement process. These uncertainty components were classified by their magnitude and origin and subsequently minimized by appropriate steps in the INAA process. The process was tested with the INAA determination of Cr in SRM 1152A stainless steel; the Cr value is certified at 17.76% with an estimated uncertainty of 0.04% (0.23% relative). The INAA results from this procedure are in agreement with these specifications. Similar procedures have been applied to INAA multi-element determinations in a high temperature alloy. Agreement with available consensus values was demonstrated in the alloy. The guidelines on the determination of uncertainty were fully met, providing through INAA a valuable independent non-destructive tool in chemical measurements of metrological value such as required in the CCQM key comparisons.     

Comparative performance of INAA and other spectroscopy techniques in the elemental analysis of stainless steel materials

Samples of high alloy Stainless Steel SS 1 were analyzed by instrumental neutron activation analysis (INAA) at 5 research institutes in 4 European countries within the frame of an Inter-Laboratory Comparison (ILC) exercise aiming at checking if the results were independent of the standardization methods, and if INAA was accurate enough to contribute to certification. The mean element concentration values yielded by INAA were also compared with mean values obtained by atomic emission spectroscopy techniques at other laboratories that took part in the International Proficiency Testing organized by KIMAB Institute of Sweden, producer of the SS 1. The performances of the nuclear and atomic techniques were compared in terms of the z-score values calculated for 11 element concentrations evaluated by the two analytical ways. Finally, consideration is given to the ways in which highest accuracy and precision can be ensured for certifying stainless steels as CRMs.     

Use of multivariate and neutron activation analysis on studying element interrelationships in Brazilian phosphorite

Methods to determine U, Th, and other constituent elements in mineral matrices through Instrumental Neutron Activation Analysis (INAA), have been widely utilized due to their capability to extract a large quantity of information from small samples. In the present work, an experimental methodology based on INAA associated to the cluster statistics technique was used to determine the uranium concentration and its correlation with other elements present in the mineral phosphorites from the northeast region of Brazil. Data for 22 elements including rare-earth elements are presented. A good correlation between uranium and rare-earth elements is observed. For the transition metals, correlation with uranium was not noted.