Determination of picogram amounts of technetium in environmental samples by neutron activation analysis

A procedure for the determination of trace amounts of ⁹⁹Tc in filter paper and vegetation samples by neutron activation analysis has been developed. The procedure consists of the following major steps: (a) pre-irradiation separation of technetium from the sample and purification of the technetium fraction; (b) thermal neutron irradiation of the ⁹⁹Tc fraction to produce ¹⁰⁰Tc ; (c) post-irradiation separation and purification of ¹⁰⁰Tc from other activated nuclides: (d) counting of the 16-sec ¹⁰⁰Tc in a low-background β-counter.

The estimated detection limits for ⁹⁹Tc by this procedure with irradiations at a thermal neutron flux of about 5.10¹³ n cm^-2 sec^-1 are: 5.lO^-12g ⁹⁹Tc in filter paper samples, and 9. 10^-12 g ⁹⁹Tc in vegetation samples.     

Determination of trace amounts of dissolved mercury compounds by instrumental neutron activation analysis following a selective preconcentration

Using an aniline sulfur resin for the selective enrichment of mercurials from surface waters it is possible to determine ppb amounts of mercury by INAA within less than three days after irradiation. Interferences from other elements, especially Na, Se, U and Au, can be avoided by following defined preconcentration and elution conditions.     

Determination of gunshot residues by neutron activation analysis

Systematic investigations of gunshot residues, deposited around the bullet hole, have been carried out. The traces were produced by firing on filter papers from distances of 5 to 200 cm using one rifle and three pistols as arms. Antimony, lead and barium were quantitatively determined after irradiating the samples in the nuclear reactor TRIGA Mainz by measurement of gamma-lines of^122mSb,¹²²Sb,^207mPo and¹³⁹Ba. The determinations were made purely instrumentally and-where the half lives were long enough-also after chemical separation of the nuclides. The amount of the elements were determined in dependence of the firing distance and of the area around the bullet hole.     

Determination of lithium by instrumental neutron activation analysis

The fast transfer system in the DR 2 reactor for irradiation at a thermal neutron flux density of 10¹³ n·cm⁻²·sec⁻¹ was used for the determination of lithium by the⁷Li(n, γ)⁸Li reaction. β-counting with a large perspex Cerenkov detector begun at 0.3 s after the end of irradiation, and multi-scaler data was accumulated in 300 channels at 0.1 s per channel. With a suitable choice of discrimination level only¹⁶N and background interfere, and the 0.84 s half-life of⁸Li was resolved by the method of weighted least squares. Results are presented for 36 international geochemical reference materials, and for a few biological samples, including BOWEN's kale and the NBS Standard Reference Material 1571 Orchard Leaves.     

Determination of iron isotopes by neutron activation analysis

Instrumental neutron activation analysis has been applied to the determination of Fe isotopic abundances in iron materials with the experimental accuracy of 5%. The proposed method can be considered as a quite simple and fast quality check system on the iron isotope enriched oxides used as standard in Mössbauer spectroscopy.     

Determining trace amounts of nickel in plant samples by neutron activation analysis

Neutron activation analysis of plant samples for trace amounts of nickel has applications in various fields. Landsberger and Robinson (Trans Am Nucl Soc 102:187–188, 2010) found their measurement of the concentrations of nickel for different NIST reference materials to be significantly greater than the certified values when measuring nickel from the 810.8 keV gamma ray that comes from ⁵⁸Co from the ⁵⁸Ni(n,p) reaction. They determined that this overestimation was due to a significant interference by the presence of ¹⁵²Eu at 810.5 keV, and presented a method for correcting this interference. Their method involved a long thermal irradiation and correction of gamma ray counts based on the 1,408 keV belonging to ¹⁵²Eu. This paper presents an alternative approach, which involves irradiating the samples with epithermal neutrons, which suppressed the ¹⁵²Eu to the point of being negligible for samples with low levels of europium. Both methods were determined to work well for the identification of nickel concentrations by neutron activation analysis.     

Determination of trace amounts of rare earth elements by neutron activation analysis after preconcentration using hydrated magnesium oxide

A preconcentration method of 13 rare earth elements (REES) was studied for neutron activation ananlysis (NAA). Hydrated magnesium oxide was used as the preconcentration agent to absorb the REES ions from aqueous solution onto the solid magnesium oxide, which was separated and analyzed. It was observed that the Langmuir equation for isothermal adsorption was well obeyed by the REES under the condition studied. The efficiency of the preconcentration process using hydrated magnesium oxide was critically examined for each of REE and for mixture of REES by preparing a known volume of solution containing known amount of trace REES. NAA was used to analyze REES recovered by the preconcentration process. It was found that the REES recoveries were satisfactory and the preconcentration process is reliable. There are several resort resort areas in Taiwan where local people are enjoying its hot spring water. It is generally believed that the hot spring water spa would bring about some sorts of therapeutic functions. The preconcentration method developed above, was applied to analyze the trace amounts of REES in hot spring wate in Taiwan.     

Determination of rhenium in molybdenites by neutron activation analysis

A thermal neutron activation method for the determination of rhenium in molybdenites is described. The rhenium is separated from the matrix after irradiation by pyridine extraction from 4 N sodium hydroxide solution; γ- and β-spectrometry are applicable. For a neutron flux of 4 · 10¹¹ n/cm².sec, an irradiation of 2 h and a sample of ca. 50 mg, β-counting allows determinations in the p.p.b. range.     

Determination of cobalt by substoichiometric thermal neutron activation analysis

A selective method has been developed for the determination of traces of cobalt in different matrices by the sensitive technique of thermal neutron activation analysis employing radiochemical separation and substoichiometric extraction of Co/II/ with iso-nitrosobenzoylacetone into chloroform.     

Determination of mercury in air by neutron activation analysis

A sensitive method for the determination of mercury in sea and surface waters is presented. A distinction is made between inorganic, organic and particulate mercury. In the determination of inorganic mercury, the element is isolated by reduction and volatilization, followed by absorption on a charcoal column. The total mercury content of the water with and without suspended solids is determined by absorption from the solution onto a column of charcoal. In all cases, the mercury on the absorber is determined by thermal neutron activation analysis. The limit of detection is l ng 1^-1.     

Determination of lithium in graphite by neutron activation analysis

Trace impurities of lithium in graphite is one of the sources of tritium in high-temperature reactors. To determine contents of less then 1ng/g a procedure based on the (n,)-reaction of⁶Li was developed. The samples are irradiated in a reactor and then ignited in a Wickbold apparatus. Thereby the tritium produced by the (n,)-reaction is completely converted in HTO, which can be easily purified by distillation and, if necessary, by a scavenger precipitation step. Several types of graphite have been investigated and the lowest content measured was 0.2 ng/g.     

Determination of mercury in bismuth by neutron activation analysis

A method has been developed for the determination of traces of mercury in bismuth by neutron activation analysis. After sample irradiation at a flux of 7 · 10¹³ n cm^-2 s^-1 for 20 min, mercury was separated from bismuth by addition of ammonium sulfide and re-dissolution of bismuth (matrix) sulfide with nitric acid, and filtration of sulfur containing mercury on a membrane filter. The activity of the 68- or 68–77-keV region, counted with a Ge(Li) or NaI(Tl) detector, was used for quantitative measurements. The method was applied to bismuth samples containing 0.1–100 p.p.m. of mercury.     

Determination of gold in platinum by neutron activation analysis

The determination of gold in platinum by neutron activation analysis is described. The possibility of screening out the influence of the nuclear reactions on the final result of the determination was studied. In the case of microamounts of gold in platinum, gold was separated previously by extraction chromatography with dithizone as organic stationary phase. Gold fixed on the column was irradiated and determined gamma-spectrometrically.     

Determination of bismuth in lead by neutron activation analysis

Neutron activation analysis for bismuth in lead was performed through the separation and measurement of²¹⁰Po, using two different extraction procedures. The reproducibility of the results was good for lead containing bismuth in higher concentrations. For high purity lead, variations in the bismuth content have been found by different analyses of the same sample, owing to inhomogeneity in the distribution of the Bi metal traces. An independent analysis of the same lead samples gave comparable Bi concentrations.     

Determination of chromium in blood by neutron activation analysis

A procedure for the determination of chromium in blood has been developed with a sensitivity of 5×10⁻³ μg Cr. Dried blood was irradiated with a neutron flux of 10¹² n·cm⁻²·sec⁻¹ in the VVRS reactor for 4 weeks, then the sample was mineralized and the chromium isolated by extraction as perchromic acid. The determination of the chromium content was accomplished by measuring the 0.32 MeV gamma energy of⁵¹Cr. In order to make correction for the interfering reaction⁵⁴Fe(n,α)⁵¹Cr, the formation of chromium from high-purity iron was investigated. The chromium content of the blood samples was between 1.03×10⁻² and 5.2×10⁻² ppm Cr.     

Determination of some precious metals by neutron activation analysis

A neutron activation procedure for the determination of Ru, Pd, Os, Ir, Pt and Au in a single irradiation in silicate rocks, meteorites and sulfide ores has been developed. An alkali fusion was used to dissolve and mix 100 to 200 mg powder samples with appropriate carriers. The individual metals were separated and brought to a state of high radiochemical purity by distillation, ion exchange and solvent extraction techniques. Precious metal activities were counted by both γ and β-methods. The procedure was evaluated by replicate analyses of the granite and diabase rock standards, G-1 and W-1 and a Cu−Ni sulfide matte which had previously been analysed by emission spectrographic and spectrophotometric methods. The results were compared with previously published data. A major discrepancy was found only for Ir in W-1.     

Determination of cadmium by substoichiometric thermal neutron activation analysis

A rapid and selective method has been developed for the determination of cadmium in environmental samples by thermal neutron activation analysis, employing substoichiometric solvent extraction technique. Alcoholic solution of 2-mercaptobenzothiazole /2-HMBT/ has been used for the substoichiometric extraction of Cd/II/ from an aqueous solution of pH 7.0 into methyl iso-butyl ketone /MIBK/.     

Determination of trace amounts of uranium in silicate materials by means of neutron activation analysis involving rapid radiochemical separation

We determined uranium in silicate materials such as standard rocks and a meteorite by radiochemical neutron activation analysis. After activation with a cadmium cover, samples were subjected to radiochemical separation of uranium immediately. The gamma-ray intensity of²³⁹U was measured with a planar type pure germanium detector system. Our data are mostly consistent with the literature or reported values. Compared with a non-destructive method, the present method was found to improve the sensitivity by at least a factor of ten. Several errors which might be involved in our RNAA procedures were examined and their degrees were evaluated.     

Determination of trace amounts of copper and selenium in biological samples by chemical separation prior to neutron activation analysis

It was found that Cu and Se can be relatively easily and accurately determined by preconcentration of Cu and Se prior to the determination by neutron activation analysis with the short-lived IRN's (Indicator Radionuclides)⁶⁶Cu and^77mSe. The method consists of wet acid digestion followed by coprecipitation with lead tetramethylenedithiocarbamate. The precipitate was collected, irradiated and counted. The validity of the method was confirmed both by internal checks, as the measurement also by⁷⁵Se and by the use of two reference material of biological origin. The limit of detection was found to be 20 ng Se and 50 ng Cu for a 0.1 g sample.     

Determination of trace amounts of mercury in water by neutron activation analysis with lubricating base oil as extractant.

This paper deals with a convenient method in the determination of trace amounts of mercury in water. After being irradiated with neutrons, water sample was treated with 7.0M HCIO4 solution and mercury was extracted with lubricating base oil. In such a simple operation, the sensitivity can reach 10(-8)g Hg/4ml H2O.