Application of prompt gamma-ray analysis and instrumental neutron activation analysis to identify the beef production distinct

We present chemometric study to identify the provenance of agricultural product, beef. Combination of instrumental neutron activation analysis (INAA) and prompt gamma-ray analysis (k ₀-PGA) were performed to determine 10 elements, C, H, N, S, Sm, Br, Mg, Na, K, Cl, nondestructively. We measured elemental profiles in beef samples produced from different districts in Japan, Australia and USA. In the case of PGA, k ₀-method was employed to determine the elemental concentrations. There was a difference in elemental profiles between Japanese black cattle beef and that produced in USA through principal component analysis (PCA). However, Holstein beef of Japan and that of Australia was not sufficiently grouped by the PCA modeling with the elemental data set. This is the first study to identify the provenance of beef through elemental analysis.     

Application of the INAA methods for KRISS infant formula CRM analysis: standardization of INAA at KRISS

We have established an instrumental neutron activation analysis (INAA) method, including k₀-based INAA, at the Korea Research Institute of Standards and Science (KRISS) for the certification of reference materials. As part of establishing INAA measurements, KRISS infant formula certified reference material was analysed for multiple elements at three different metrological institutes: KRISS and NIST for the standard comparator method, and JSI for the k₀-INAA method. The mass fraction of most elements was consistent within expanded uncertainty (k?=?2). In addition, the results were used to verify the validity of elemental analysis of Zn using the standard comparator INAA at KRISS, and spreadsheet-based INAA calculations were evaluated.

     

Monitoring of environmental contaminants: 10 years of application of k0-I INAA

Examples of the application of k ₀ standardized instrumental neutron activation analysis (k ₀ -INAA) to aerosols and biological monitors in the last 10 years at Instituto Tecnológico e Nuclear (ITN) are given. As an analytical technique, INAA, in association with the k ₀ method was applied to these materials in four different projects, aiming at monitoring concentrations of heavy metals and others elements in the atmosphere in the Portuguese territory. In these studies we analysed the lichen Parmelia sulcata Taylor and olive tree bark as monitors as well as aerosol samples. For each project some representative results are presented, followed by a discussion of the application of this technique to environmental studies.     

Measurement and evaluation of k0 factors for PGA at JAERI

In order to determine multiple elements by k ₀ standardization-based neutron induced prompt gamma-ray analysis (PGA), measurements and evaluation of k ₀ factors for the elements have been performed. The k ₀ factors using Cl as a comparator for 27 elements, which are effective for the analysis by PGA, were measured with precision almost less than 3% using the cold and thermal guided neutron beams at JRR-3M. The accuracy of the k ₀ factors were better than 10% except for the non-1/v elements of Cd and Sm. Neutron spectrum correction is necessary for common use of k ₀ factors of the non-1/v 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.     

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.     

Trace elements in the water cycle of the Šalek valley,Slovenia, using INAA

Three watersheds were studied by sampling bulk precipitation deposition, seepage water at 50 cm soil depth and spring water. As the main analytical method for determination of trace elements and heavy metals in water samples, thek ₀-based method of INAA was used. The results showed an increased content and concentration range of trace elements in precipitation, soil water and spring water in the vicinity of the otanj Thermal Power Plant. We demonstrated that thek ₀-based method of INAA as a multielement nondestructive technique is a highly suitable approach to determining some toxic trace elements in environmental studies of the water cycle.     

k0 Standardization Approach in Neutron-Induced Prompt Gamma-Ray Analysis at JAERI

The k ₀ standardization method has been studied and applied at JAERI for the accurate determination of multielements by neutron-induced prompt gamma-ray analysis (PGA). The k ₀ factors for 26 elements using Cl as a comparator were measured by the cold and thermal neutron guided beams of JRR-3M with an uncertainty less than 3% except for a few elements. The k ₀ factors for most elements obtained with both cold and thermal neutrons agreed within 3%, and agreed also with those measured at other cold and thermal neutron guided beams within 10%, except for a few elements. Multielement determinations in reference materials were performed using the k ₀ factors obtained to evaluate the accuracy and precision of this work.     

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%.     

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.     

Comparison of relative INAA and k 0-INAA using soil and sediment reference materials

The objective of this work was to compare the results obtained by the relative INAA and k ₀-INAA methods for the same input parameters (sample mass, nuclear data, net peak area for the same gamma line and the same measurement and same cooling and measurement times). In total eight environmental soil and sediment reference materials (RM) or certified reference materials (CRM) from different producers were analysed. In this work only the recommended or certified values were considered, allowing comparison of the two methods for 30 elements. The results point out that k ₀-INAA possesses superior qualities compared to relative INAA, being insensitive to flux gradients, and independent of recommended/certified values in RMs/CRMs, often used as standards in relative INAA.     

Application of k0-based internal mono standard instrumental neutron activation analysis method method for composition analysis of stainless steel clad sample

The k₀-based internal mono standard instrumental neutron activation analysis (INAA) method was used for the composition analysis of some irregular shape stainless steel (SS) samples of type SS 316M, which is used as fuel cladding in Indian fast breeder test reactor (FBTR). The method utilizes in situ relative detection efficiency using γ-rays of the activation products present in the sample for overcoming γ-ray self-attenuation. Samples were neutron activated using the thermal column as well as the core position of the reactor and the assay of radioactivity was carried out by high-resolution gamma ray spectrometry. The elements determined were Fe, Cr, Ni, Mo, Mn, Co, Cu, As and W. Since all the major elements (Fe, Cr, Ni, Mo and Mn) were amenable to NAA, the relative elemental concentrations with respect to Fe, obtained by this method, were converted to their absolute values by mass balance. The results were compared with specified compositions and found to be satisfactory. In order to validate these results obtained by the standard-less approach, sub samples of SS 316M in solution forms were analyzed by prevalent relative and k₀ methods of INAA, and results were found to be in good agreement. The accuracy of the internal mono standard INAA method has been evaluated by analyzing an alloy steel certified reference material, CRM 225/1 of British Chemical Standards (BCS).     

Determination of <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript>-values for some elements in neutron capture gamma-ray for prompt gamma activation analysis

Exploration and modification of data for k ₀-PGAA (prompt γ-ray activation analysis) values used as standards for k ₀ standardization are needed. An integrated system has been installed and calibrated in Hot Laboratories Center for PGAA, using ²⁵²Cf isotopic neutron source with neutron flux of 6.16E8 n/cm² s. The prompt k ₀-factors of about 12 elements were determined versus the 1951.1 keV γ-ray of the ³⁵Cl, as well as analyzing crude oil and oil product samples. The concentrations of the elements in crude oil H, B, Mg, Al, Na, Si, P, S, Cl, V and Cd were 1.18E5, 0.084, 5.48E2, 8.45E2 4.88E2, 1.62E2, 3.72E2, 8.2, 144.3, 393 and 209.2 ppm while in oil product samples were 1.32E5, 5.87, 4.56E2, 4.22E2, 7.16E3, 699, 157, 8.74, 492.3, 61 and 198.2 ppm. Validation of the k ₀-PGAA was applied in analyzing standard IAEA reference material (soil-7) which give good agreement with the literature data. The ²⁵²Cf neutron beam in radiation position was characterized by the cadmium-ratio method, and found that the cadmium ratio (f), was 160.     

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.     

Performance evaluation of k 0-instrumental neutron activation analysis and flame atomic absorption spectrophotometry in the characterization of various types of alloys

Certified alloys of Ni–Cu based, Fe based and Cu–Sn based were analysed by semi-absolute, standardless k ₀-instrumental neutron activation analysis (k ₀-INAA) and flame atomic absorption spectrophotometry (FAAS) aiming at evaluating their comparative performances. In k ₀-INAA measurements, the irradiations were performed at miniaturized neutron source reactor having thermal neutron flux of about 1 × 10¹² cm^?2 s^?1. The experimentally optimized parameters for INAA suggested a maximum of three irradiations for the quantification of 21 elements within 5 days. The same experiments also produced quantitative results of 13 elements not reported in the certificates of the reference materials. AAS was, however, unable to determine any of those elements. Accuracy of the two techniques was assessed by comparing their average root mean squared errors. The data analysis concluded that k ₀-INAA had better sensitivity and accuracy than FAAS.     

Characterisation of some exotic fruits (Morus nigra, Morus alba, Salvadora persica and Carissa opaca) used as herbal medicines by neutron activation analysis and estimation of their nutritional value

In the under developed countries, the people of far-flung rural areas still depend to a large extent upon herbal medicines. At the foundation of usage of herbal medicine is the experience of thousands of years. The present paper deals with the characterisation of exotic fruits for essential and toxic elements. The samples include Morus nigra, Morus alba, Salvadora persica and Carissa opaca (from low and high altitude). Two standardizations of neutron activation analysis, that is, semi-absolute k ₀-instrumental neutron activation analysis (k ₀-INAA) and epithermal neutron activation analysis (ENAA) were employed for the quantification of elements. The analysis methodologies were validated by analyzing the IAEA-336 (lichen) and NIST-SRM-1572 (citrus leaves). Sixteen elements including Br, Ca, Cl, Co, Cr, Fe, I, K, Mg, Mn, Na, Rb, Sb, Sc Sr, and Zn were determined in all samples. Daily intakes of various elements from the samples were measured and compared with the dietary reference intakes. Additionally, principal component analysis was performed to extract information regarding samples and elements.     

Development of the <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript>-based cyclic neutron activation analysis for short-lived radionuclides

The k ₀-based cyclic neutron activation analysis (k ₀-CNAA) technique has been studied to explore the applicability at the Portuguese research reactor (RPI). In particular, for the determination of elements which form short-lived radionuclides, particularly fluorine (²⁰F, 11.16 s half-life) and selenium (^77mSe, 17.36 s half-life) in polymer, biological and environmental samples. The detection limits obtained for F and Se were about 50 and 0.01 mg kg⁻¹, respectively, in the investigated materials. The timing parameters for the procedure were 10 to 20 s for irradiation, 5 s decay, 10 to 20 s counting, 5 s waiting and performed with eight cycles. The k ₀-IAEA program was modified to use millisecond time resolution for irradiation, decay and counting times as needed for interpreting k ₀-CNAA data in terms of concentration, accuracy and detection limit. The quality control of the procedure was performed by preparing a standard solution containing fluorine with different contents as well as using the certified reference materials containing selenium from which the bias between the results and the certified values were within 15% for most elements at the investigated content ranges. The analytical results for several other elements producing short-lived or detectable radionuclides, e.g., Al, Ca, Cl, Cu, Dy, I, Mg, Mn, Ti, and V were also obtained by the k ₀-CNAA procedure with accuracy within 12%.     

INAA and PIXE for the determination of the contents of extractable sediment

The three-stage BCR sequential step reference extraction procedure was applied to the reference material BCR CRM 601, especially developed for fractionation studies. Extracted fractions were analyzed for Cr, Ni, Zn, Cd, and Pb, by k ₀-standardized instrumental neutron activation (k ₀ INAA) and proton induced X-ray emission (PIXE), and flame atomic absorption spectrometry (FAAS). Sample preparation procedures were developed for both k ₀ INAA and PIXE techniques, related to the evaporation of the solutions in order to get solid samples for neutron and proton irradiation. Quality control was assessed by intercomparison of the analytical results obtained by the applied techniques, which included results for a few certified reference materials. In the extracted fractions, chromium concentration was not determined accurately by both nuclear techniques. Concerning Cd, Ni, Pb, and Zn, the results were in general in good agreement with the certified values and FAAS. Some incomplete separation of the residue might have occurred.     

Multi-element analysis of soil from the north-western region of India by neutron activation analysis using the single comparator method with special reference to selenium toxicity

The single comparator (k₀) instrumental neutron activation analysis (INAA) was employed to determine the elemental composition of soil from the north-western region of India. The radiometric assay was carried out using high resolution gamma-ray spectrometry. Seventeen elements were detected including selenium whose concentration was found to be in the range of 1.02 to 6.79 mg/g.     

Comparison of the catalogues of thek 0-and thek Zn single comparator methods for standardization in INAA

The independently measured catalogues of two single comparator methods for standardization in INAA, i.e., thek _Zn-and thek ₀-method, were compared. Many reactions were listed only in thek _Zn-catalogue; in these cases other literature data were used to supplement thek ₀-catalogue. The agreement between thek _Zn-and thek ₀-catalogue was found to be much better than the agreement between thek _Zn-catalogue and other literature data. It is therefore suggested to use the convertedk _Zn-catalogue as a supplement of the previously publishedk ₀-catalogue.