Instrumental neutron activation analysis of environmental samples using thek 0-standardization method

The use of thek ₀-standardization method in instrumental neutron activation analysis gives good accuracy and precision. The analysis time can be reduced drastically by employing software for thek ₀-standardization calculations. In this work samples were irradiated in a TRIGA reactor and the gamma spectrum was analysed by Sampo 90 and thek ₀-standardization by the KAYZERO/SOLCOI code (DSM Research). The efficiency measurement and the peak to total ratio at the reference and other geometries were measured and tested for their accuracy by analysing some reference materials. Reference materials such as SRM 1572 (Citrus leaves), SRM 1573 (Tomato leaves), SRM 1575 (Pine needles), IAEA Soil-7 (Soil) and SRM 1646 (Estuarine sediment) were analysed for the major, minor and trace element contents. The results were in good agreement with the certified or literature values. The recently released IAEA 140 (Sea plant homogenates) was also analysed for 28 elements.     

k 0-INAA of biological matrices at IPEN neutron activation analysis laboratory,São Paulo,using the k0_IAEA software

This study presents the results obtained in the application of the k ₀-standardization method at the Neutron Activation Analysis Laboratory at IPEN (LAN-IPEN), for biological sample analysis, by using the k0_IAEA software, provided by the International Atomic Energy Agency (IAEA). The thermal to epithermal flux ratio f and the shape factor α of the epithermal flux distribution of the IEA-R1 nuclear reactor of IPEN were determined for the pneumatic irradiation facility and one selected irradiation position, for short and long irradiations, respectively. To obtain these factors, the “bare triple-monitor” method with ¹⁹⁷Au–⁹⁶Zr–⁹⁴Zr was used. To evaluate the accuracy of the results, bias (%) and E _n-number test were applied to the results obtained in the analysis of the biological reference materials NIST SRM 1547 peach leaves, INCT-MPH-2 mixed polish herbs and NIST SRM 1573a tomato leaves. Bias (%), for most elements, ranged from 0 to 30 %, in relation to certified values. E _n-number values showed that, with few exceptions (Na in NIST SRM 1547 and NIST SRM 1573a, and Al, Cr, Sc and Zn in INCT-MPH-2), the results were within a 95 % CI. These results pointed to the possibility of using the k ₀-INAA method with the k0_IAEA software for analysis of biological samples at LAN-IPEN.     

Neutron activation analysis of reference materials by the k0-standardization and relative methods

Instrumental neutron activation analysis with the k₀-standardization method was applied to eight geological, environmental and biological reference materials, including leaves, blood, fish, sediments, soil and limestone. To a first approximation, the results were normally distributed around the certified values with a standard deviation of 10%. Results obtained by using the relative method based on well characterized multi-element standards for IAEA CRM Soil-7 are reported.     

Contents of arsenic, mercury and other trace elements in Napoleon's hair determined by INAA using the k0-method

Two samples of Napoleon's hair were received for determination of arsenic, mercury and other trace elements by INAA. Before sample irradiation, the hairs were washed following the IAEA washing procedure. Two standard reference materials of GBW09101 (human hair) and NIST/SRM1572 (citrus leaves) were analyzed along with Napoleon's hair for quality control. Standardization was conducted by applying the k ₀-method implemented in the program MULTINAA. The contents of arsenic and mercury as well as three additional elements chromium, antimony and zinc in Napoleon's hair are reported. Compared to the present normal levels, all of the determined elements in Napoleon's hair, except the mercury, are found to be irregular.     

The k0-method in cold-neutron prompt gamma-ray activation analysis

The k ₀-standardization method has been applied and evaluated at the cold-neutron prompt gamma-ray activation (PGA) facility of the Swiss spallation source SINQ (Paul Scherrer Institute). The k ₀-factors for 26 elements of interest were measured using chlorine as a comparator. The results showed good agreement with the values determined at other cold and thermal neutron guided beams, except for a few elements. Then, standard reference materials were analyzed to assess the accuracy of the method using the obtained k ₀-factors. Finally, the technique was used for multielement determination in various samples coming from nuclear waste storage, geochemistry and geology. In addition, the non-destructive nature of PGAA offered an interesting application in archeology.     

Implementation of the k 0-standardization method for analysis of geological samples at the Neutron Activation Analysis Laboratory, São Paulo, Brazil

The Neutron Activation Analysis Laboratory (LAN-IPEN) has been analysing geological samples for many years with the INAA comparative method, for geochemical and environmental research. This study presents the results obtained in the implementation of the k ₀-standardization method at LAN-IPEN, for geological samples analysis, by using the program k ₀-IAEA, provided by the International Atomic Energy Agency (IAEA). The thermal to epithermal flux ratio f and the shape factor α of the epithermal flux distribution of the IEA-R1 nuclear reactor of IPEN were determined for the pneumatic irradiation facility and one selected irradiation position, for short and long irradiations, respectively. To obtain these factors, the “bare triple-monitor” method with ¹⁹⁷Au–⁹⁶Zr–⁹⁴Zr was used. In order to validate the methodology, the geological reference materials basalts JB-1 (GSJ) and BE-N (IWG-GIT), andesite AGV-1 (USGS), granite GS-N (ANRT), SOIL-7 (IAEA) and sediment Buffalo River Sediment (NIST–BRS-8704), which represent different geological matrices, were analysed. The concentration results obtained agreed with assigned, with bias <10 % except for Zn in AGV-1. The U-score test showed that all results, except Mg in JB-1, are within 95 % confidence interval. These results indicate excellent possibilities of using this parametric method at the LAN-IPEN for geochemical and environmental studies.     

Determination of total mercury in environmental and biological samples using k0-INAA, RNAA and CVAAS/AFS techniques: Advantages and disadvantages

The accuracy and precision of the results obtained for total mercury in various environmental and biological samples and certified reference materials (CRMs) by various analytical methods, including k ₀-instrumental neutron activation analysis (k ₀-INAA), radiochemical neutron activation analysis (RNAA) and cold vapour atomic absorption (and atomic fluorescence) spectrometry (CVAAS/AFS) used in routine analysis in our laboratory, were investigated. Three natural matrix reference materials (RMs) from the International Atomic Energy Agency (IAEA), five CRMs from the Institute for Reference Materials and Measurements (IRMM), six CRMs from the National Institute of Standards and Technology (NIST) and one from the Jožef Stefan Institute (IJS) were analyzed. The results obtained show good agreement between certified or assigned values, and between the methods used, except for some data obtained by k ₀-INAA in biological samples. This can be explained by losses during irradiation in semi-open systems (irradiation in plastic ampoules) and/or spectral interferences. This revised version was published online in August 2006 with corrections to the Cover Date.     

Assessment of three digestion procedures for Zn contents in Pakistani soil by flame atomic absorption spectrometry

Evaluation of three different digestion procedures for accurate determination of elemental concentration in soils was undertaken. The digestion procedures, two leaching and a total dissolution processes were compared for twenty-one soil samples. The soil standard reference materials (SRMs), IAEA Soil-5 and IAEA Soil-7 were analysed for quality control purposes. Zinc (Zn) was analysed using flame atomic absorption spectrometry (FAAS). Precise analysis was accomplished in the SRM and soil samples, which was better than 4.7% for leaching and total dissolution procedure. Compared with the elemental concentration in soil samples, HF–HClO₄ procedure achieved greater accuracy, where as HNO₃–H₂O₂ and HNO₃–H₂SO₄–HCl procedures were comparable with slight variation in a few samples.     

Instrumental neutron activation analysis of Moroccan geological samples using the k0-standardization method

Instrumental neutron activation analysis (INAA) for traces and major elements of several geological samples from “Zgounder” region in Morocco was performed utilizing the k ₀-standardization method. Sample irradiation has been done by the 250 kW Triga Mark II reactor at Jozef Stefan Institute in Slovenia. Due to its accuracy, sensitivity and specificity, the k ₀-standardization method is the most suitable method for non-destructive multielement analysis mainly for trace elements in rocks. It requires an accurate knowledge of the parameters of the irradiation facilities and other instrumentation parameters. It is an absolute standardization method, where the absolute nuclear data are replaced by a nuclear constant, the k ₀-factor, determined experimentally with high accuracy. More than 40 elements were determined using about 30-second short and about 7-hour long irradiations. Gamma-rays emitted from the irradiated samples have been determined by a high purity germanium detector. Accuracy was assessed using the standard reference material AGV-1. This was less than 1% for major elements and about 5% for traces. This revised version was published online in July 2006 with corrections to the Cover Date.     

k0-NAA quality assessment by analysis of different certified reference materials using the KAYZERO/SOLCOI software

A suite of natural matrix reference materials (RMs) were used to assess the quality of analytical results obtained by k ₀-instrumental neutron activation analysis (k ₀-INAA) at the Joef Stefan Institute (IJS). Five certified reference materials (CRMs) from the Institute for Reference Materials and Measurements (IRMM), two standard reference materials (SRMs) from the National Institute of Standards and Technology (NIST), three RMs from the International Atomic Energy Agency (IAEA) and one RM from IJS were analyzed. Altogether, results for twenty-four elements in inorganic matrices and twenty-nine elements in organic matrices, obtained by k ₀-INAA, were compared to certified values. Results obtained show good agreement with certified or assigned values except for Fe, La, Nd, Sm and U in inorganic matrices, and Ag, Al and Cr in organic matrices.     

Element concentrations in candidate biological and environmental reference materials by ko-standardized INAA

Summary k_o-Based Neutron Activation Analysis (k_oINAA) was used to analyze the candidate reference materials Apple Leaves and Peach Leaves, and Oriental Tobacco Leaves and Virginia Tobacco Leaves. Concentration values for 27 elements were measured. The accuracy was ascertained by analysis of two certified reference materials, NIST 1572 Citrus Leaves and 1573 Tomato Leaves. The homogeneity test of the IAEA Evernia prunastri candidate reference material in aliquots 100 mg is extended to the elements Sc, Cr, Fe, Co, Zn, Rb, Sb, Cs, Ba, Ce and Th.     

Application of NAA standardization methods using a low power research reactor

Two widely used neutron activation analysis (NAA) standardization methods (relative and k ₀) have been validated at the Ghana Research Reactor-1 (GHARR-1) Centre using environmental and biological standard reference materials (SRMs). The samples were IAEA Soil-7 as an environmental sample, and NIST Orchard Leaves 1571 as a biological sample. The qualitative and quantitative analyses were done using a high resolution Canberra N-type high purity germanium (HPGe) detector. The accuracy and precision were evaluated for the elements analysed. The concentrations of most of the elements were found to be within 10% of the certified values. Precision was calculated from six replicate measurements and was found to be within 15%.     

Accuracy and precision in instrumental neutron activation analysis of reference materials and lake sediments

The k₀-standardization method applied in instrumental neutron activation analysis depends on experimental parameters such as the calibration of the detector and the metrology of the irradiation position. The related systematic errors are evaluated; Student's t-test is applied to results obtained for reference materials by the k₀-method. Precision is estimated for the reference materials and routine lake sediments by a method suggested by Minkkinen based on duplicate measurements.     

Multielement comparison of instrumental neutron activation analysis techniques using reference materials

Several instrumental neutron activation analysis techniques (parametric, comparative, and k_o-standardization) are evaluated using three reference materials. Each technique is applied to National Institute of Standards and Technology standard reference materials, SRM 1577a (Bovine Liver) and SRM 2704 (Buffalo River Sediment), and the United States Geological Survey standard BHVO-1 (Hawaiian Basalt Rock). Identical (but not optimum) irradiation, decay, and counting schemes are employed with each technique to provide a basis for comparison and to determine sensitivities in a routine irradiation scheme. Fifty-one elements are used in this comparison; however, several elements are not detected in the reference materials due to rigid analytical conditions (e.g., insufficient length of irradiation or activity for radioisotope of interest decaying below the lower limit of detection before counting interval). Most elements are normally distributed around certified or consensus values with a standard deviation of 10%. For some elements, discrepancies are observed and discussed. The accuracy, precision, and sensitivity of each technique are discussed by comparing the analytical results to consensus values for the Hawaiian Basalt Rock to demonstrate the diversity of multielement applications.     

The feasibility of utilizing the64Cu annihilation 511 keV line in INAA

This work demonstrates that the⁶⁴Cu 511 keV line can be used in INAA to determine trace amounts of Cu in biological and environmental materials. The method to reduce the serious interference in γ-ray spectroscopy from nuclides having high energy γ-rays is discussed. A simple INAA procedure is proposed and examined for 7 different SRM materials. An accuracy and precision better than 3% are achieved for tested samples with Na-to-Cu content ratio less than 1000. The minimum detectable Cu concentrations of less than several ppm are calculated for all the analysed samples. To retain the multi-element capability, the k₀-and the modified monostandard methods are applied by using the⁶⁴Cu 511 keV line as the comparator. With the aid of the program MULTINAA, maximum 32 elements are simultaneously determined with an accuracy better than 5% for most elements.     

Establishing a basis for nuclear archaeometry in Australia using the 20 MW OPAL research reactor

The k ₀-method of standardisation for instrumental neutron activation analysis (INAA) has been used at the OPAL research reactor to determine the elemental composition of three certified reference materials: coal fly ash (SRM 1633b), brick clay (SRM 679) and Montana soil (SRM 2711). Of the 41 certified elements in the three materials, 88 percent were within five percent of the certified values and all determinations were within 15 percent of the certified values. The average difference between the measured and certified values was 0.1 percent, with a standard deviation of 4.1 percent. Since these reference materials are widely used as standards in the analysis of archaeological ceramics by INAA, it has been concluded that the INAA facility in Australia is particularly well-suited for nuclear archaeometry.     

Installation of Kayzero-INAA standardization in the TNRC and its applications for trace elements determination in different materials

The paper focuses on the validation of the k ₀-method of instrumental neutron activation analysis (k ₀-INAA) in the Tajura Nuclear Research Center (TNRC) via the analysis of several certified reference materials. The selected reference materials were: SRM 1572 Citrus Leaves, SRM 1575 Pine Needles, IAEA-A11 Milk Powder, IAEA-V-10 Hay Powder, RM IAEA-Soil-7 and RM IAEA-SL-1 Lake Sediment. The method is based on the PC version Kayzero/Solcoi software package issued by DSM. All the samples, reference materials and monitors were irradiated in various positions of the Tajura reactor with different f and α. The parameters f and α (f — thermal/epithermal neutron flux ratio, α — parameter accounting for the non-ideality of the 1/E epithermal neutron fluence rate distribution) were determined using the bare triple monitor method. The results obtained for all the reference materials are in good agreement with the certified values.     

Determination of trace elements in cigarette tobacco with the <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript>-based NAA method using Es-Salam research reactor

The k ₀-standardization method of NAA is known as one of the most remarkable progress of NAA with its many advantages. Recently, our laboratory is highly involved in various areas of application of k ₀-NAA. This paper focuses on the application of the k ₀-NAA method in Nutritional and Health-Related Environmental field. Tobacco holds a leading position among different commodities of human consumption. The adverse health effects of toxic and trace elements in tobacco smoke on smokers and non-smokers are a special concern. In the present study, the concentration of 24 trace elements in cigarette tobacco of five different brands of Algerian and American cigarettes have been determined by k ₀-based INAA method. The results were compared with those obtained for samples from Iranian, Turkish, Brazilian and Mexican cigarettes tobacco. To evaluate the accurate of the results the SRM IAEA-140/TM was executed. The analytical results showed that the relative error of most of the elements was less than 10%.     

Reactor power dependency of the neutron flux parameters fork 0-standardization

Using the facilities of the Triga Mark III reactor at the NNRI, Mexico and the HAV-1 multipurpose monitor, the reactor power dependency for thek ₀-standardization essential neutron flux parameters as: epithermal shape factor (), thermal to epithermal ratio (f) and neutron temperature (T _n ) were experimentally obtained. Evaluation of the obtained dependencies shows that it is unnecessary to analyze the possible introduction of correction factors in thek ₀-INAA experimental results. A single experimental procedure to determine throughf is suggested.     

Accelerating <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript>

Combining the powers of a fast pneumatic transport system and the Automatic Activation Analyzer (AAA) of the Atominstitut in Vienna with the newest version of the IAEA k ₀-Software, the application of the k ₀-method to the determination of short-lived radionuclides becomes easily possible. By calculating Asp-values with the IAEA software, the often expensive and time-consuming measurement of Asp-values using certified reference materials is reduced to quality control checks. Measurements clearly show that the two approaches are equivalent, especially since both take self-absorption and neutron self-shielding into account. In this way it is possible to expand the library of the AAA with many hitherto unobtainable Asp-values. At the same time, using highly accurate Asp-values already measured for many short-lived radionuclides, k ₀-values for those can be produced with a simple procedure.