Use of enriched <Superscript>74</Superscript>Se and <Superscript>77</Superscript>Se in combination with isotope pattern deconvolution to differentiate and determine endogenous and supplemented selenium in lactating rats

A quantitative methodology has been developed to differentiate between endogenous and supplemented selenium in lactating rats using two enriched selenium isotopes. Lactating rats were fed for 2 weeks with formula milk containing one enriched Se isotope, ⁷⁷Se, as the metabolic tracer. The isotopic composition of selenium in serum and urine samples was then measured by collision cell ICP-MS after the addition of a solution containing another enriched isotope, ⁷⁴Se, as quantitation tracer, before analysis. Isotope pattern deconvolution allowed the transformation of measured Se isotopic abundances into concentrations of natural abundance (endogenous) selenium and enriched ⁷⁷Se (supplemented) present in the samples. The proposed methodology was validated using serum and urine reference materials spiked with both ⁷⁷Se and ⁷⁴Se. The obtained results are discussed in terms of selenium exchange and half-life in lactating rats (11–12 days) and selenium levels in serum in comparison with non-supplemented rats and control rats after maternal feeding.     

Determination of selenium in food matrices by replicate sample neutron activation analysis

The replicate sample instrumental neutron activation method was optimized and used for the determination of selenium in foodstuffs. The method was reliable, yielding accurate results. Lower detections limits were obtained after each successive irradiation. Different irradiation conditions were used depending on the type of sample. For samples with higher selenium contents (meat, fish, eggs), the measured selenium in the first replicate is in all cases larger than the detection limit, but a better accuracy was obtained with a larger number of replicates (2–3 replicates). For samples with extremely low selenium contents (vegetable samples), at least seven replicates were necessary to obtain a concentration value two times larger than the detection limit.     

Measurement uncertainty of iodine determination in radiochemical neutron activation analysis

The measurement uncertainty of iodine determination in NIST standard reference material (SRM) 1549 using radiochemical neutron activation analysis (RNAA) was studied. This method is based on ignition of the irradiated sample [¹²⁷I(n,)¹²⁸I, t_1/2=25 min, E=422.9 keV] in an oxygen atmosphere, followed by absorption of iodine in a reducing acid solution and its purification by a selective extraction–stripping–reextraction cycle. The purified solution of iodine in CHCl₃ was transferred to a well-type HPGe detector for -ray measurement of the induced radionuclide ¹²⁸I. The detection limit of the method employed under the conditions described was 1 ng/g. The reproducibility of iodine determination in the SRM was 3.6% (12 determinations within 1 month), calculated by the analysis of variance procedure. Using the commercially available software program GUM Workbench and the recommendations of the Eurachem/CITAC Guide, we evaluated the uncertainty budget for this RNAA method and the relative uncertainty obtained was 3.6%. The largest uncertainty contributions were due to the repeatability of the chemical yield determination, the count rate of the induced nuclide in the standard and sample, the mass of the carrier and the mass of the irradiation standard.     

Progress in neutron activation analysis for uranium

A new type of extractant, sym-dibenzo-16-crown-5-oxyhydroxamic acid (HL) is introduced. The extractions of UO22+, Na+, K+, Sr2+, Ba2+ and Br- were studied with HL in chloroform. The results obtained show that UO22+ can be quantitatively extracted at pH values above 5, whereas the extractions of K+, Na+, Sr2+, Ba2+ and Br- are negligible in the pH range of 2 - 7. The dependence of the distribution ratio of U(VI) on both the concentration of the HL and pH are linear, and they have the same slope of 2. This suggests that U(VI) appears to form a 1:2 complex with ligand. Uranium(VI) can be selectively separated and concentrated from interfering elements such as Na, K, Sr and Br by solvent extraction with HL under specific conditions. The recovery of uranium is nearly 100% and the radionudear purity of uranium is greater than 99.99%. Therefore, neutron activation analysis has greatly improved the sensitivity and accuracy for the detection of trace uranium from seawater.     

Evaluation of <Superscript>40</Superscript>K in vegetables collected Malaysia by determination total potassium using neutron activation analysis

Some vegetables of important nutritive requirements have been collected from Kuala Lumpur region capital of Malaysia. The vegetables were analyzed in order to determine activity concentration level of potassium using neutron activation analysis (NAA). The NAA results obtained showed the activity concentration of ⁴⁰K varied from 379 Bq/kg (Egg-plant) to 1585 Bq/kg (Spinach Red). These results are compared to other researches and are clear that the concentrations of K are relatively high in the Malaysia in compared to rather than vegetables of Pakistan and Jamaican. However, they are seen not to pose any serious internal health burden due to ingestion given the realities of vegetables choice by individuals in the study area.     

A combined method of neutron activation analysis and radiometric measurements for <Superscript>234</Superscript>U and <Superscript>238</Superscript>U determination in soil samples of low uranium concentration

A method that combines the use of non-destructive neutron activation analysis and high-resolution α spectrometry has been developed for determination of the activities of ²³⁴U and ²³⁸U in geological samples of low uranium content. The ²³⁸U content is determined by k₀-based neutron activation analysis, whereas the ²³⁴U/²³⁸U relationship is measured by α spectrometry after isolation and electrodeposition of the uranium extracted from a lixiviation with 6 M HCl. The main advantage of the method is the simplicity of the chemical operations, including the fact that the steps destined to assure similar chemical state for the tracer and the uranium species present in the sample are not necessary. The method was applied to soil samples from sites of the North Peru Coast. Uranium concentration range 3–40 mg/kg and the isotopic composition correspond to natural uranium, with about 10% uncertainty.     

Accurate measurement of bromine contents in plastic samples by instrumental neutron activation analysis

Accurate measurements of bromine contents in plastic samples were made by the direct comparator instrumental neutron activation analysis (INAA). Individual factors affecting the measurements were comprehensively evaluated and compensated, including the volatility loss of bromine from standard comparators, the background bromine level in the filter papers used for preparation of the standard comparators, nuclear interference, γ-ray spectral interference and the variance among replicates of the samples. Uncertainty contributions from those factors were thoroughly evaluated and included in the uncertainty budgeting of the INAA measurement. ⁸¹Br was chosen as the target isotope, and the INAA measurements for bromine were experimentally confirmed to exhibit good linearity within a bromine content range of 10–170 μg. The established method has been applied to the analysis of eight plastic samples: four commercially available certified reference materials (CRMs) of polyethylene and polystyrene and four acrylonitrile butadiene styrene (ABS) samples prepared as the candidate reference materials (KRISS CRM 113-01-012, -013, -014 and -015). The bromine contents of the samples were calculated at three different γ-ray energies and compared, showing good agreement. The results of the four CRMs also showed good consistency with their certified values within the stated uncertainties. Finally, the bromine contents of the ABS samples were determined with expanded uncertainties (at a 95% level of confidence) between 2.5% and 5% in a bromine content range of 25–900 mg kg⁻¹.     

Validation of the determination of tin by <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript>-instrumental neutron activation analysis in foodstuff

Several recent intercomparisons and certification exercises have shown that the determination of tin in e.g. food samples and plastics is not straightforward. k ₀-Instrumental Neutron Activation Analysis (k ₀-INAA) offers some intrinsic quality control opportunities for the determination of the tin content in samples since several monitoring radioisotopes are formed. In this work we will discuss the validation of the determination of tin by k ₀-INAA using different reference materials. The results show that only few of these radioisotopes are reliable in terms of accuracy and that from a survey of the tin content in a range of canned foods detection limits as low as 2 mg/kg can be achieved.     

Enzymatic probe sonication extraction of Se in animal-based food samples: a new perspective on sample preparation for total and Se speciation analysis

This paper describes a fast, simple and novel extraction method for total selenium and selenium species determination in food samples. Parameters influencing extraction, such as sonication time, extracting media, temperature, sample mass, ultrasound amplitude and sample/enzyme mass ratio were investigated. The enzymatic hydrolysis proposed, enhanced by probe sonication, allowed the quantitative extraction of selenium in chicken muscle, liver, kidney and feed (97, 93, 95 and 102%, respectively) in 2 min, maintaining the original Se-species integrity. Total Se content of the samples was determined using inductively coupled plasma mass spectrometry. Se-species were identified and quantified using high-performance liquid chromatography in conjunction with inductively coupled plasma mass spectrometry. Chromatographic analyses were carried out under two chromatographic conditions and led to the identification of SeMet in all samples. The accuracy of the proposed method was assessed using certified reference materials as well as microwave digestion. Potential advantages of the proposed method over traditional hydrolysis are speed, simplicity and safety of the procedure.     

SDAT: analysis of <Superscript>131m</Superscript>Xe with <Superscript>133</Superscript>Xe interference

The Spectral Deconvolution Analysis Tool (SDAT) software was developed at The University of Texas at Austin. SDAT utilizes a standard spectrum technique for the analysis of β–γ coincidence spectra. Testing was performed on the software to compare the standard spectrum analysis technique with a region of interest (ROI) analysis technique. Experimentally produced standard spectra and sample data were produced at the Nuclear Engineering Teaching Laboratory (NETL) TRIGA reactor. The results of the testing showed that the standard spectrum technique had lower errors than the ROI analysis technique for samples with low counting statistics. In contrast, the ROI analysis technique outperformed the standard spectrum technique in high counting statistics samples. It was also shown that the standard spectrum technique benefitted from a compression of the number of channels within the spectra.     

Characterization of purified <Superscript>241</Superscript>Am for common impurities by instrumental neutron activation analysis

Americium is an important actinide element having versatile applications based on its alpha and gamma emissions. Multi-element determination of radioactive samples using ICP-AES technique may be affected by the presence of americium due to its rich emission spectra. With a view to characterize plutonium based fuels containing americium for trace metals by ICP-AES technique accurately, a high purity ²⁴¹Am (using a separation procedure developed in our laboratory) was prepared. To ascertain its chemical purity it is essential to determine its impurity contents accurately. Instrumental neutron activation analysis (INAA), being a sensitive multi-elemental technique, was employed to determine the concentrations of impurities in purified ²⁴¹Am. Detection limits for the common elements and rare earth elements have also been determined. Comparison is made with the analytical data obtained by the ICP-AES method.     

Determination of radionuclidic impurities in <Superscript>99m</Superscript>Tc eluate from <Superscript>99</Superscript>Mo/<Superscript>99m</Superscript>Tc generator for quality control

Technetium-99m is the principal radioisotope used in medical diagnostics; radionuclidic impurity is the major concern of its quality. This work presents a analytical method for sequential determination of all radionuclidic impurities listed in pharmacopoeia including gamma emitters, alpha emitters, ⁸⁹Sr and ⁹⁰Sr. Radioactive decay for removal of ^99mTc, ion exchange and extraction chromatography for removal of ⁹⁹Mo and ⁹⁹Tc are effective for separation of interferences. Gamma spectrometry, LSC with alpha/beta discrimination, and Cherenkov counting using LSC are sensitive methods for measurement of the impurity radionuclides. The detection limits of this method are well meet the requirement of the quality control according to the limitation of the pharmacopoeia.     

Combined determination of <Superscript>99</Superscript>Tc and <Superscript>108m</Superscript>Ag in L/ILW liquid wastes

The low- and intermediate-activity level liquid wastes produced by the Paks Nuclear Power Plant (NPP) contain routinely measureable gamma-emitting (e.g., ⁵⁴Mn, ⁶⁰Co, ^110mAg, and ¹³⁷Cs) as well as many so-called “difficult-to-measure” radionuclides. Despite of their low specific activity compared to the total, the reliable determination of these radionuclides is an important issue of nuclear waste management. The increasing amount of waste samples to be qualified yearly by our laboratory put a pressure on revising the existing procedure of ⁹⁹Tc separation applied. We have managed to halve the initial amount of the sample required to achieve the same level of detection of technetium. Furthermore, one of the new purifying steps introduced have proved to be able to separate ^108mAg (and ^110mAg) better than 99% keeping the ⁹⁹Tc content of the product almost intact. Means of separation of ⁹⁹Tc from ¹⁰⁶Ru and ^124+125Sb have also been successfully investigated. As intended, this new procedure has a major impact on the chemical reagent as well as the electricity requirement of the separation making it more cost-effective.     

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.     

Non-destructive assay technique for the determination of <Superscript>238</Superscript>U/<Superscript>232</Superscript>Th ratio in the mixed oxides of uranium and thorium using prompt gamma-ray neutron activation

A non-destructive assay technique based on prompt gamma-ray neutron activation analysis for the determination of ²³⁸U to ²³²Th ratio in the mixed oxide fuel materials has been established. The method uses closely spaced high energy gamma-rays in the region of 4000 keV to 4150 keV enabling it to be applied for samples of any geometry and thickness without having any correction for gamma-ray attenuations and detection efficiencies.     

<Superscript>226</Superscript>Ra and <Superscript>228</Superscript>Ra determination in environmental samples by alpha-particle spectrometry

A complete methodology for ²²⁶Ra and ²²⁸Ra determination by alpha-particle spectrometry in environmental samples is being applied in our laboratory using ²²⁵Ra as an isotopic tracer. This methodology can be considered highly suitable for the determination of these nuclides when very low absolute limits of detection need to be achieved. The ²²⁶Ra determination can be performed at any time after the isolation of the radium isotopes from the analyzed samples while the ²²⁸Ra determination needs to be carried out at least six months later through the measurement of one of its grand-daughters. The method has been validated by its application to samples with known concentrations of these Ra nuclides, and by comparison with other radiometric methods.     

Application of instrumental neutron activation analysis to ceramic solid electrolytes

Beta" alumina isomorphs with different conducting cations were produced by ion exchange in molten salts. The concentration of the main component (Al), of conducting ions (Na⁺, Sr⁺⁺, Ba⁺⁺) and of chlorides from residues of the melt inside the exchanged material was determined by instrumental neutron activation analysis (INAA).Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

Short- and long-time neutron activation analysis of egyptian phosphate reference materials

Three Egyptian phosphate reference materials (S1, S2 and S3) were investigated using short-term activation analysis. The precision of the determination of Dy, Sc, Gd, Yb, Mg, V, F, Al, Mn, and Ca by this method ranged from 2 to 5% due to the homogeneity factor. Another 11 elements were determined by NAA using medium and long-lived nuclides. Most results were in good agreement with the recommended values. The values of Dy and Gd are reported.     

Rapid measurement of selenium in biological samples using instrumental neutron activation analysis

A rapid instrumental system for measuring selenium via 17 second^77mSe has been applied to the analysis of a wide variety of biological specimens encountered in biomedical research. The reliability and versatility of the method is documented for serum and animal tissue specimens. Analysis results for SRM 1577 bovine liver show excellent accuracy and precision.