Multielement neutron activation analysis of biological materials using chemical group separation and Ge(Li) gamma spectrometry

Neutron activation analysis (NAA) for the determination of some trace elements in biological materials is described. The method presented permits the simple and rapid determination of Se, Ag, Au, Sb, Pt (via¹⁹⁹Au), Hg, Co, Ni (via⁵⁸Co), Fe, Zn, Mo, Sn, Cr, Cd, Cu and As after radiochemical separation from Na, K, Cs, Rb and partially Br. For this purpose, postirradiation separation by extraction with mercury or zinc amalgam was used. Separation of gold by extraction with ethyl acetate or by precipitation with dimethylglyoxime was applied for the determination of gold and platinum in biological materials.     

A comparison of neutron activation analysis and inductively coupled plasma mass spectrometry for trace element analysis of biological materials

Fifty individual food types were analysed by instrumental and radiochemical neutron activation analysis as well as inductively coupled plasma mass spectrometry after testing all techniques by analysing IAEA mixed human diet, H-9. The performance of these trace element techniques and their limitations were evaluated under normal, routine, multi-element surveys of a large range of solid biological materials.South Australian Department of Agriculture, 21 Divett Place, Adelaide, SA, Australia.     

Ge(Li) gamma-ray spectrometry as a pilot for NaI(Tl) gamma-ray spectrometry

Lithium-drifted germanium semiconductor detectors give much better resolution than do thallium-activated sodium iodide detectors, but much lower sensitivity. They can often advantageously be used in conjunction with NaI(Tl) detectors, to show whether corrections must be applied for activities other than the one to be measured and to provide the necessary information for calculation of the corrections.     

Application of neutron activation analysis for trace element determinations in biological materials

Over the past three decades, more and more interest has been focused on trace eleemnts in biological materials. This increasing interest has gone hand in hand with the continuous improvement of analytical techniques. Neutron activation analysis has proven to be a most suitable method for the quantitative determination of a wide variety of trace (0.01–100 μg g^?1) and ultratrace (<0.01 μg g^?1) elements in biological materials. This technique has even played a preponderant role in this field.     

Analysis for the rare-earth elements by neutron activation and Ge(Li) spectrometry

A procedure for analysis of 12 of the rare-earths, tested on more than a hundred samples of rocks and minerals, is described. Carrier is added for each element to be determined. Samples are fused with Na₂O₂. The rare-earths are separated as a group, then precipitated and mounted as oxalates for Ge(Li) spectrometry. Following radioassay, chemical yields for the individual rare-earths are obtained by irradiation and counting of the carrier. About two months are needed to obtain complete data for a set of four samples, but many samples are analyzed concurrently. The precision and accuracy exceed ±5 per cent for 10 of the elements in 0.1 to 0.5 g samples of common rocks.     

A program for complete quantitative neutron activation analysis using Ge(Li) detector gamma spectrometry and a small computer

It is shown that the large sophisticated programs designed for big computers can be efficiently used on medium scale machines for complete quantitative neutron activation analysis with Ge(Li) detectors.     

Radiochemical separation for the certification of some trace elements in biological reference materials by neutron activation analysis

A radiochemical separation procedure based on chromatographic separation using Chelex-100 in 0.1M HAc-0.1M NH₄Ac at pH 4.8 and TDO in 6M HCl, has been developed to determine Cd, Co, Cr, Fe, Se, The, U, W and Zn in three biological materials of botanic origin used as SRM's: 1547 Peach Leaves, 1515 Apple Leaves and the new proposed material Spinach. The aim was to obtain more information for these elements whose values are not yet determined or are given only as suggested values.     

A definitive method for the determination of trace amounts of cobalt in biological materials by neutron activation analysis

A new, very accurate (definitive) method for the determination of trace amounts of cobalt in biological materials has been devised. The method is based on combination of neutron irradiation with quantitative and selective post-irradiation separation of cobalt from all accompanying radionuclides followed by measurement by -ray spectrometry. Column chromatography in which owing to addition of Co carrier the course of separation can be followed visually is the key element of the separation scheme. Several criteria have been formulated which must be simultaneously fulfilled in order to acknowledge the result as obtained by a definitive method. The high accuracy of the method has been demonstrated by the analysis of several certified reference materials of widely different Co contents.     

A two-group separation scheme for the determination of eleven trace elements in biological material by neutron activation analysis.

The applicability of solvent extraction with tri-n-octylphosphine oxide (TOPO) in the neutron activation analysis of biological material has been studied. A two-group radiochemical separation scheme is presented. After wet oxidation, As, Se, and Hg are removed by distillation and subsequent sulfide precipitation; Ca, Cd, Co, Fe, Mo, Sc, W, and Zn are then determined after extraction with TOPO. Chemical yield is determined for the volatile group by re-irradiation of the sulfide precipitate. No chemical yield determination is performed for the TOPO group. Results for six international biological standards are presented. The method is applicable to a wide variety of biological samples.     

Thallium determination in biological materials by radiochemical neutron activation analysis

Summary The determination of thallium in biological materials sometimes cause problems because of the low concentrations of this toxic element. In the present work a method is described which optimizes the parameters affecting the specificity and sensitivity of the radiochemical NAA of thallium in biological samples. High thermal neutron flux, complete decomposition of the organic matter by pressurized digestion, TlI precipitations, liquid extraction of HTlBr₄ and La(OH)₃ scavenging purification are the steps leading to the final homogeneous preparation of Tl₂CrO₄ for -activity measurement. The method was applied to various materials as bovine liver, bone and nails. Good agreement was found between certified and determined thallium concentrations of the reference material CRM 176. The chemical yield comes to about 80%, with low deviations. The sensitivity of the method is about 10^–3 g/g, the standard deviations being in the range of 3.6% (CRM 176), 14% (bovine liver), and 17% (bone). Detailed working instructions are given.     

Neutron activation analysis determination of all 14 stable rare-earth elements with group separation and Ge(Li) spectrometry

A lithium-drifted germanium detector, 40 cm³, combined with a radiochemical group separation, has been utilized to determine the concentrations of 14 stable rare-earth elements in a silicate rock sample, following thermal-neutron activation. Thirteen rare earths could be determined within an 8-day decay period. The remaining rare-earth element (Tm) required a longer delay, and subtraction of the interfering contribution from¹⁶⁰Tb. Samples of standard rock G-1 and W-1 were also analyzed by this procedure for 13 rare earth elements, results of which are compared with literature values.     

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.     

Some practical procedures in computerized thermal neutron activation analysis with Ge(Li) gamma-ray spectrometry

The practical use of a correction procedure for random coincidence losses, the determination of the detection limit and the standardization of measuring conditions are described. Special correction methods for the interference of the Cu analysis by²⁴Na, the burn-up of the radioactive nuclide formed and the interference of the Pt determination by Au are also given.     

Multielement trace analysis by atomic absorption spectrometry and neutron activation analysis in biological matrices

According to calculations of NIX and others, the formation of superheavy elements might occur in heavy-ion reaction systems such as the one under investigation in the present work i.e.,²³⁸U+^63,65Cu at 9.6 MeV/nucleon. Since previous experiments have indicated that upper limits to the production cross-section for superheavy elements are extremely low, we have carried out two rather long irradiations of 27 hrs and 42 hrs, respectively, at the University of Manchester LINAC. The first run has already been reported on in the literature. In the case of the second run, after chemical separation into HgS, CdS, and La(OH)₃ fractions, the samples were assayed simultaneously and continuously over a period of 6 months for alpha-and spontaneous-fission activity, using Si surface-barrier detector. Each sample was at the same time mounted on mice, for the purpose of scanning for fission tracks at a later date. No indications from the data have so far been found that superheavy elements were produced.     

Radiochemical separation and determination of europium by Ge(Li) detector in biological tissues

A simple neutron activation method has been developed for the determination of europium in biological tissues and applied in the analysis of marine organism samples with ±9% precision at the nanogram level. The method is based on the separation, by ion-exchange, of the rare earth group from dry or ashed irradiated tissues and subsequent determination of^152mEu, by γ-spectrometry using a lithium drifted germanium detector.^152mEu, separated almost completely from other than rare earth elements, with better than 98% chemical yield, is counted on the 121.8 keV photopeak which then is practically free from any other γ-ray energy interfering in this counting.     

Low-level determination of silicon in biological materials using radiochemical neutron activation analysis

Summary A new radiochemical neutron activation analysis (RNAA) method has been developed for low-level determination of Si in biological materials, which is based on the ³⁰Si(n,γ)³¹Si nuclear reaction with thermal neutrons. The radiochemical separation consists of an alkaline-oxidative decomposition followed by distillation of SiF₄. Nuclear interferences, namely that of the ³¹P(n,p)³¹Si with fast neutrons, have been examined and found negligible only when irradiation is carried out in an extremely well-thermalized neutron spectrum, such as available at the NIST reactor. The RNAA procedure yields excellent radiochemical purity of the separated fractions, which allows the measurement of the β^--activity of the ³¹Si by liquid scintillation counting. Results for several reference materials, namely Bowen’s Kale, Bovine Liver (NIST SRM 1577b), Non-Fat Milk Powder (NIST SRM 1549) and several intercomparison samples, Pork Liver-1, Pork Liver-2 and Cellulose Avicel, are presented and compared with literature values.     

A pre-irradiation separation procedure based on ion-exchange chromatography for gallium determination in biological and environmental materials by neutron activation analysis

A pre-irradiation separation procedure, for gallium determination in biological and environmental materials by neutron activation analysis (NAA) is reported. The proposed method, based on ion-exchange chromatography, allows to eliminate the radiation risk, while taking the advantages of high sensitivity of NAA. The single comparator method is employed for gallium quantitative evaluation. Since no standard reference materials with certified gallium contents were available, the reliability of the proposed method was extensively investigated by various approaches. Four biological and one environmental standard reference materials, with gallium contents ranging from 54 g/g-3 ng/g, have been analyzed.     

Trace element analysis of biological materials by thermal and epithermal neutron activation analysis

A scheme for instrumental neutron activation analysis of biological materials is proposed. The scheme is based on a combination of thermal and epithermal activation. The accuracy is evaluated by analyzing 4 standard reference materials. Results from the analysis of human blood serum and plasma are given.