Determination of palladium in different samples by neutron activation after selective preconcentration with α-benzildioxime

A procedure is described for the determination of submicrogram quantities of palladium in sea water, biological and geological materials. Palladium is preconcentrated by coprecipitation with α-benzildioxime at pH 2 in the presence of citric acid followed by neutron activation. The method is highly selective and only traces of other metals are adsorbed on the surface of the precipitate. The instrumental variant of counting of long-lived ¹⁰⁹Pd (t$\text{1}\text{2}$ = 13.6 h) after 16-h irradiation gives a detection limit of 10 ng. A further decrease of the detection limit to 1 ng can be attained by removal of radioactive impurities (mainly ²⁴Na, ⁵⁶Mn and ⁸²Br) after washing the dichloromethane extract of dissolved precipitate with an aqueous solution of citric acid containing inactive carriers of bromide, manganese and sodium ions. Palladium (¹⁰⁹Pd) is finally measured by a NaI(Tl) well type scintillation detector. The method can be applied to most environmental samples.     

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.     

Determination of selenium in human diets by radiochemical neutron activation analysis.

A post-irradiation radiochemical separation technique was tested for the determination of selenium levels in diet samples, collected by using a duplicate portion technique, from both rural and urban population groups in Turkey. The technique involved sample irradiation, acid digestion, selective distillation, precipitation and filtration steps. During the separations it was possible to determine the yield of each sample using a stable selenium carrier. An average chemical yield of 71 +/- 3% was obtained for the radiochemical neutron activation analysis. For samples from urban and rural regions, the average selenium concentrations obtained were 0.14 +/- 0.04 and 0.07 +/- 0.02 mg kg-1, respectively. It was also possible to determine daily dietary selenium intakes, which were found to be 81 +/- 41 micrograms and 23 +/- 11 micrograms for the urban and rural groups, respectively. Although daily selenium intakes were found for a small number of subjects in this study, the separation technique developed can be used for determination of the selenium status in larger population groups.     

Determination of chromium in aquatic environment by substoichiometric thermal neutron activation analysis

Chromium has been determined in environmental samples. The method described here involves the irradiation of environmental samples and a g quantity of standard with thermal neutrons at the self-serve position in the CIRUS reactor, followed by dissolution of the sample and standard in the presence of a milligram amount of carrier. Both the sample and the standard are subjected to substoichiometric extraction under controlled experimental conditions with alizarin into cyclohexane. An aliquot of the organic phase was counted on a gamma-ray spectrometer. The concentration of Cr in water samples from Bombay and Karad City, and the accuracy, precision and sensitivity of the method are discussed.     

Rapid determination of selenium in various marine species by instrumental neutron activation analysis

Instrumental neutron activation analysis was used to determine selenium concentrations in several marine organisms including two certified reference materials /NRCC lobster hepatopancreas, NBS oyster tissue/ and one uncertified material /IAEA fish homogenate/. The⁷⁶Se/n, /^77mSe/T=17.4 s/ reaction was successfully employed to achieve an overall precision between 3–10% and detection limits between 0.3–0.6 g/g. The accuracy of the results, as compared to the certified values, was in excellent agreement with the NBS material and only slightly lower /9%/ for the NRCC material.     

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 all platinum-group elements in mantle derived xenoliths by neutron activation analysis with NiS fire-assay preconcentration

A modified NiS fire-assay neutron activation method is developed for the determination of all platinum-group elements (PGEs) in mantle-derived xenoliths. This method is characterized by sub-ppb detection limits, <0.1~0.002 ppb procedural blanks and 7~15% analytical precision for PGEs. Analyses of PGE standard rocks indicate that this modified NiS fire-assay neutron activation method is as reliable as the method previously proposed for a large scale of samples. The capability of the method for the measurement of PGEs in the upper mantle is also illustrated by some exciting results obtained from mantle-derived xenoliths of Eastern China.     

Fractionation analysis of iodine in bovine milk by preconcentration neutron activation analysis

Iodine is an essential trace element for human beings. The main source of iodine is generally food items such as fish and milk. Either the lack or the excess of iodine can cause health problems. There exists an increasing interest in the determination of total iodine as well as various species of iodine in milk. We have developed an epithermal neutron activation analysis method with a Compton suppression (ENAA-CS) counting system for the determination of ng mL⁻¹ levels of iodine. We have also employed chemical separation methods prior to ENAA-CS to measure the fraction-specific concentrations of iodine in bovine milk. We have measured the following iodine concentrations in homogenized milk (3.25%milk fat): 0.48 ± 0.02 μg mL⁻¹ of total iodine, 0.020 ± 0.003 μg mL⁻¹ of lipid-bound iodine, 0.039 ± 0.002, 0.019 ± 0.002 and 0.021 ± 0.004 μg mL⁻¹ of protein-bound iodine depending on the protein separation method and 0.45 ± 0.02 μg mL⁻¹ of inorganic species.     

Determination of selenium(IV) and selenium(VI) in natural water samples by neutron activation analysis after chemical pre-collection

Neutron activation analysis using shortlived^77mSe (T=17.5 s) preceded by chemical pre-collection of Se on activated carbon (AC) has been applied to the fractional determination of Se(IV) and Se(VI) in natural water samples such as river water and sea water. Two chemical procedures were adopted: adsorption of Se(IV)/Bismuthiol-II complex on AC and adsorption of Se(VI)/Bismuthiol-II on AC after reduction of Se(VI) to Se(IV). It was shown that Se(IV) and Se(VI) can be determined at a <g l^–1 (ppb) level in natural waters by the present method.     

Determination of mercury in human urine by neutron activation analysis,with lead diethyldithiocarbamate as a preconcentration agent

Lead diethyldithiocarbamate is an effective reagent for preconcentration of mercury in urine for neutron activation analysis. Sodium and bromine are removed from the sample by this procedure. As lead diethyldithiocarbamate is insensitive to neutron activation, radiochemical separation is not needed after neutron irradiation. Results from the analysis of urine collected from workers in caustic soda manufacturing plants are discussed.     

Rapid determination of selenium in erythrocytes by neutron activation analysis

The use of ultrafiltration prior to the determination of selenium via the short-lived activation product,^77mSe, provided a simple and rapid method for the determination of this element in erythrocytes. An associated reduction in analytical error made this procedure acceptable for monitoring small changes in erythrocyte selenium concentrations.     

The determination of chromium in water samples by neutron activation analysis after preconcentration on activated carbon

A method is presented for the determination of chromium in sea-and fresh water. Chromium is concentrated on activated carbon from neutral solution after a previous reduction of chromate with sodium sulfite at pH 1.5. The final determination of the total chromium content is performed by instrumental neutron activation analysis. By preconcentration on activated carbon a differentiation between tervalent and hexavalent chromium is possible. A separate determination of both species is not yet feasible due to the high carbon blank and to the necessity of measuring the adsorption percentage on carbon. The lower limit of determination, which depends on the value of the carbon blank, is 0.05 μg Cr·1⁻¹ with a precision of 20%.     

Determination of trace copper in water samples by neutron activation analysis preceded by preconcentration on activated carbon powder

To determine trace copper in water samples such as tap and rain water, neutron activation analysis preceded by chemical preconcentration was developed, in which copper was concentrated by adsorption on activated carbon powder using 8-quinlinol as an adjunct. Short-lived⁶⁶Cu and long-lived⁶⁴Cu were used as analytical radionuclides. It was demonstrated that copper can thus be detemined at a μg l⁻¹ (ppb) level.     

Determination of selenium in nickel and cobalt concentrates applying epithermal neutron activation analysis

The physicochemical association of plutonium in soil near the Subsurface Disposal Area (SDA) at the Idaho National Engineering and Environmental Laboratory (INEEL) has been determined using selective sequential extraction techniques. Our results suggest that plutonium in surface soils is associated primarily with the hydrous oxide coatings of the soil (37±5.3%). Appreciable amounts of plutonium were also removed with the organic matter (22±2.8%) and carbonates (13±3.1%). On the other hand it appears that plutonium association with the soluble and exchangeable components of the soil is relatively small (>4.0%). The remainder of plutonium (21±4.7%) is tightly bound to the refractory silicate residue of the soil. Relatively little plutonium is available for physicochemical mobilization from the soil under the present prevailing conditions of the INEEL site.     

Rapid determination of selenium in human serum by neutron activation analysis

A simple and rapid method was developed for the determination of selenium in human serum using a pre-irradiation separation technique of ultrafiltration followed by neutron activation analysis via the short-lived activation product^77mSe. The method was validated using certified reference material.     

Determination of gold in natural waters by neutron activation and γ-spectrometry after preconcentration with tributyl phosphate as solid extractant

A method for the preconcentration of gold in natural waters at the sampling site using tributyl phosphate as a solid extractant [Se(TBP)] was developed as a preliminary step prior to the determination of gold by neutron activation and γ-spectrometry. The SE(TBP) was saturated with gaseous chlorine for extracting all gold species. In batch experiments gold was quantitatively retained on the SE(TBP) in 10 min. After extraction and washing, the SE(TBP) was ashed or back-extracted. Gold was quantitatively eluted with hot, neutral 0.025 M thiourea. The gold content of residues of ashing or eluents after evaporation was determined by neutron activation and γ-spectrometry. The detection limit for the overall procedure was 0.2 ng 1^?1. The efficiency was tested on ‘equilibrated’ solutions prepared from river water and tracer solutions of gold. For comparison, the gold content of natural water samples was determined using preconcentration on activated charcoal.     

Determination of seven trace elements in natural waters by neutron activation analysis after preconcentration with 1-(2-pyridylazo)-2-naphthol

A procedure is described for the preconcentration of Cd(I), Co(II), Cr(III), Cu(II), Mn(II), U(VI) and Zn(II) from 800 ml of water and sea-water samples by coprecipitation with 1-(2-pyridylazo)-2-naphthol (PAN) prior to neutron activation. Chromium is reduced to Cr(III) by hydroxylammonium chloride at pH 4 before the preconcentration step. Coprecipitation of 30 mg of PAN was most effective at pH 9 with final recoveries of 76–91% for six elements and 50% for uranium. The scheme is based on double irradiation of the same samples. Short (10 min) irradiation followed by γ-spectrometry counting for 10 min gives data for Cd (^111mCd), Co, Cu, Mn and U (²³⁹U). A second 16-h irradiation permits determination of zinc and uranium (²³⁹Np) after a waiting time of 6 h, cadmium (¹¹⁵Cd) after 24 h and chromium after a waiting period of 2 weeks followed by counting for 30 min. Detection limits are 0.04 ng g^?1 for Co, 0.8 ng g^?1 for Cd, 0.3 ng g^?1 for Cu, 0.2 ng g^?1 for Cr, 0.006 ng g^?1 for Mn, 0.006 ng g^?1 for U and 0.3 ng g^?1 for Zn. A further decrease of the detection limit for chromium to 0.05 ng g^?1 can be achieved by separation of interfering nuclides and scintillation counting of ⁵¹Cr with a NaI(Tl) well-type detector.     

Speciation of some trace elements in water samples after preconcentration on activated carbon by neutron activation analysis

A new filtering column has been developed on the covalent attachment of chelating functionalities to simple, highly hydrophilic adsorbent material, which can then complex heavy metal ions irreversibly and targeted towards toxic metals removal. The capacity of the chemically modified sorbent (modified charcoal) materials used in this work was evaluated for the above mentioned heavy metal ions in the presence of iron ions and simulated water samples. The methods are based on preconcentrations of the elements of interest on activated carbon and zirconium loaded activated carbon using specific conditions of pH and oxidation states followed by a final determination by neutron activation analysis (NAA). It has been investigated that zirconium loaded activated carbon is able to adsorb As (V), Se (VI), Cr (VI) and Hg (II) at any pH while activated carbon is able to adsorb As (III), Se (IV), Cr (III) and Hg(I) at higher pH. This revised version was published online in August 2006 with corrections to the Cover Date.