Determination of rare-earth elements in steels by radiochemical neutron activation analysis

For the separation of rare-earth elements from steel, with a cation exchange resin, separation experiments were performed on NIST reference materials of SRM-363 and SRM-364. Iron, Na, Cr, Mn, Co, Cu, As, Mo, Sb and W were separated in 2M hydrochloric acid, five rare-earth elements, La, Ce, Pr, Nd and Sm and three other elements, Hf, Zr and Ba were separated using 8M nitric acid. Each element was determined by a single comparator method using two monitors, gold and cobalt.     

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.     

Determination of gold in biological materials by radiochemical neutron activation analysis

A radiochemical neutron activation analysis procedure was developed for the determination of trace amounts of gold in biological materials. The procedure was realized with irradiation of reference and test samples in a nuclear reactor, selective and quantitative separation of gold using inorganic MnO₂ Resin and gamma-ray spectrometric measurement of ¹⁹⁸Au. The method is characterized by a low limit of detection of gold at ng g^?1 level. Results shows that the method can be applied to the determination of trace amounts of gold in tissues for medical research.     

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.     

Simultaneous determination of mercury and selenium in biological materials by radiochemical neutron activation analysis

A simple and sensitive radiochemical neutron activation analysis (RNAA) method has been developed for the simultaneous determination of mercury and selenium in biological materials. The radiochemical procedure is based upon the digestion of irradiated samples with sulphuric and nitric acids followed by subsequent extractions of mercury and selenium into toluene, first of mercury from 7.5 M H₂SO₄-0.01M HBr media and after of selenium from 7M H₂SO₄-1 M HBr media. After washing of the organic phases with similar media, the mercury bromide was back-extracted into 0.034M EDTA in 5% aqueous ammonia and the selenium bromide into 0.14M H₂O₂ in aqueous solution. The¹⁹⁷Hg and the⁷⁵Se were counted on a Ge(Li) detector. The precision and accuracy of the method was checked by analysing NBS Standard Reference Materials: orchard leaves and bovine liver.     

Nickel determination in biological materials at ultratrace level by fast neutron radiochemical activation analysis

Using radiochemical separation of cobalt following the fast neutron reaction⁵⁸Ni(n, p.)⁵⁸Co and long high fluence irradiation, we attempted to improve the determination limit for Ni to the nanogram and sub-nanogram level. A Compton suppression spectrometer was shown to be the best choice compared to co-axial or well-type HPGe detectors. Results for low level biological reference materials such as serum and milk powder are discussed. Use of both dried and pre-ashed samples showed that losses of Ni and Co on ashing are non-significant. The influence of the silica ampoule blank was also investigated.     

Determination of ten trace elements in meteorites and lunar materials by radiochemical neutron activation analysis

A procedure is reported for the determination of Ni, Ge, Ru, Au, Ir, Zn, Ga, Cd, In and U in meteorites and lunar materials. The precision in multiple determinations at the 95% confidence level is less than 10% except for gold (15%). Ruthenium and uranium are determined by counting ⁹⁷Ru and ¹⁰³Ru x-rays; the chemical yield is determined from ¹⁰⁶Ru added before sample dissolution. The activity of ^116mIn is determined with improved sensitivity from integral counts in the region 1.5–3.0 MeV on a NaI(TI) detector.     

Determination of trace elements in biological materials by instrumental epithermal neutron activation analysis

The use of reactor epithermal neutrons in instrumental activation analysis is described for the determination of trace elements via long-lived isotopes. A boron carbide filter is used. Results of analyses of human erythrocytes, plasma, urine and some biological reference materials are given to demonstrate the applicability of the method to biological samples. Bromine, iron, cesium, rubidium, selenium and zinc and cobalt are determined. The method provides accuracy and reliability similar to conventional thermal neutron activation but is faster. Limits of detection attainable with the two techniques are compared.     

Determination of 25 elements in biological standard reference materials by neutron activation analysis

Trace element analysis has been carried out on standard biological reference samples such as bovine liver, orchard and tomato leaves. Computer aided instrumental neutron activation analysis and, in some cases, preliminary chemical group separation followed by NAA were used. For Ca, Mg, Ni and Si special chemical separation and Cerenkov counting were applied. *** DIRECT SUPPORT *** A1353068 00003     

Trace determination of nickel (and cobalt) in biological reference materials by radiochemical neutron activation analysis

Summary Very few biological reference materials are certified for nickel below 1 mg · kg^–1. Neutron activation analysis was only rarely considered as a possible approach; reported sensitivities were usually not very good, unless preconcentration was applied.In the present work, the relatively high fast neutron flux of our TRIGA reactor was used to induce the ⁵⁸Ni(n, p)⁵⁸Co reaction, and ⁵⁸Co (E =811 keV) was radiochemically separated from other radionuclides by classical anion-exchange chromatography in hydrochloric acid. ⁵⁷Co was added to the irradiated sample before decomposition as a radioisotopic yield monitor. By concentrating the final sample fraction and measurement in a well-type HP Ge detector, Ni concentrations down to the 10-g · kg^–1 level could be determined for samples irradiated for 1 day. ⁶⁰Co, produced by neutron capture on ⁵⁹Co, is also coseparated and quantified from the gamma spectrum, so that both elements Ni and Co are determined. Results are reported for a series of NBS and other biological reference materials in the concentration range 10 g-10 mg · kg^–1. Possibilities for further increases in sensitivity are discussed.

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Spurenbestimmung von Nickel (und Cobalt) in biologischen Referenzmaterialien durch radiochemische Neutronenaktivierungsanalyse

     

Determination of Fe and Zn in biological samples by radiochemical neutron activation analysis

Radiochemical NAA methods have been developed for the simultaneous determination of Fe and Zn in biological samples. The method involves reactor irradiation, dissolution in 3M HCl and solvent extraction followed by counting on a scintillation gamma-ray spectrometer. Iron was separated with aqueous cupferron and extracted into chloroform while Zn was extracted with 2-thenoyl trifluoroacetone (TTA) into methyl isobutyl ketone (MIBK). Reaction conditions such as pH and the effect of solvents and various ions were studied using tracer activities. The methods have been employed for trace level determination of Fe and Zn in NBS, SRMs, Bowen's Kale, IAEA CRMs and other plant leaves.     

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.     

Ultratrace determination of platinum in biological materials via neutron activation and radiochemical separation

A neutron activation analysis scheme based upon a radiochemical separation of the activation products has been developed. The method utilizes the inherent sensitivity of the activation reaction¹⁹⁸Pt(n, γ)¹⁹⁹Pt and counting of the daughter nuclide¹⁹⁹Au. This nuclide is radiochemically separated from interfering activities by homogeneous precipitation as elemental gold. The remaining interference of the secondary reaction¹⁹⁷Au(n,γ)¹⁹⁸ Au(n,γ)¹⁹⁹Au from gold in the samples is quantitatively assessed and corrected. During this process accurate gold concentrations in the samples are obtained at ultratrace levels. The analysis scheme is applied to gold and platinum determinations in biological Standard Reference Materials and human liver specimens. Gold and platinum are determined at concentrations of 5·10^?11 g/g, and at higher levels.     

Determination of individual rare earth elements in Vietnamese monazite by radiochemical neutron activation analysis

Radiochemical neutron activation analysis (RNAA) has been applied for determination of rare earth elements (REE) in Vietnamese monazite. The chemical separation procedure used is based on the chromatographic elution of rare earth groups, after the separation of²³³Pa(Th) in irradiated monazite samples by coprecipitation with MnO₂, the rare earth elements were retained by Biorad AG1×8 resin column in 10% 15.4M HNO₃-90% methanol solution. The elution of heavy rare earth (HREE) and middle rare earth (MREE) groups was carried out with 10% 1M HNO₃-90% methanol and 10% 0.05M HNO₃-90% methanol solution, respectively; while the light rare earths (LREE) were eluted from the column by 0.1M HNO₃ solution. The accuracy of the method was checked by the analysis of granodiorite GSP-I and the rare earth values were in good agreement.     

Fast neutron activation analysis of rare-earth elements in monazite from Korea

The relative ans single comparator methods have been applied to determine 7 rare-earth elements and U, Th in Korean Monazites by 14.5 MeV neutron activation analysis. The (n, 2n) nuclear reactions are used for all elements except La, for which (n, p) reaction is used. Al is used as a flux monitor for the relative method and as a singlle comparator for the single comparator method. The analytical results obtained by the two methods agree well within 3% deviation except for Sm and Gd. These results are also compared with the result obtained by a single comparator method using reactor neutron.     

Determination of iodine in biological materials by neutron activation analysis

A method of determination of iodine (total and PBI) in serum, urine and other biological materials has been developed. The method consists in a gamma-spectrometric measurement of¹²⁸I activity after its radiochemical separation. The radiochemical separation procedure includes wet decomposition of the samples in a nitric acid medium followed by a few separation steps, the essential step being the substoichiometric extraction of iodide with a chloroform solution of tetraphenylarsonium chloride. Owing to the application of the substoichiometric separation, a high radiochemical purity of the separated iodine is achieved and the determination of the yield of radiochemical separation is not necessary.