The determination of some trace elements in rainwater by neutron activation analysis

A routine method for the determination of 12 elements in small rain water samples is presented. Instrumental neutron activation analysis is applied for the determination of Mn, Na, Cl, V and Al. Bromine and iodine are isolated by isotope exchange between the irradiated water and a solution of Br₂ resp. I₂ in CCl₄. Extraction with APDC/MIBK is used for the separation of the shortlived isotopes of Co, V, Cr, Zn and In.     

Concentration-data of elements in liquid fuel oils as obtained by neutron activation analysis

The selection of exciting source both from the point of view of excitation efficiency and elimination of matrix effects using incoherently scattered radiation from the analyzed sample is discussed. Samples of materials from the flotation process of copper ore have been used and copper, iron and lead were the elements sought. For the excitation of fluorescence X-rays, sealed radioisotopic sources of²³⁸Pu,²⁴¹Am,²⁴⁴Cm,¹⁰⁹Cd and a molybdenum X-ray tube were used. For X-ray analysis a Si(Li) spectrometer was applied. The processing of X-ray spectra based on the application of the Gaussian peak representation gives results equivalent to the total peak area method. From the intensities of fluorescence and scattered radiation, the contents of elements were calculated using empirical formulae and the results were compared with those of the Heinrich-Rasberry method. A statistical analysis of the results has been carried out and the criteria of optimal regression formula selection are given.     

Precise determination of rare earth elements in rocks by neutron activation analysis

A pre-irradiation group separation method has been developed for the neutron activation analysis of rare earth elements (REE) and Ba in silicate rocks. REE and Ba were quantitatively separated from other elements by cation exchange column method. The chemical yield of each separation was monitored with Pr added to the sample powder before decomposition. The accuracy and precision were tested by repeated analyses of JB-1 and one analysis of BCR-1. In addition, it was found that REE distribution in a granitic rock powder was inhomogeneous and therefore special care must be taken for the sampling of granitic rock powders.     

Wet-chemical analysis and determination of trace elements by neutron activation in meteorites

As a contribution to the cosmochemical distribution of elements, 35 meteorites of the collections of the Museum of Natural History in Vienna, the Mineralogical-Petrographical Institute and the Analytical Institute of the University of Vienna were analyzed. In the meteorites main and minor constituents were determined by wet-chemical methods, whereas for the determination of about 16 trace elements neutron activation analysis was employed. This paper has been dedicated to Prof. Dr.J. W. Breitenbach on the occasion of his 60th birthday.     

Determination of trace elements in some Nigerian vegetable based oils by neutron activation analysis

The concentrations of some essential micronutrient elements leadingto short-lived activation products in four Nigerian vegetable based oils (palmoil, palm kernel oil, sheabutter and groundnut oil) have been determined byneutron activation analysis using a small research reactor. One sample ofeach material was analysed and presented as an introduction for further investigations.Results indicate that the concentration range of the elements are 19.4–44.0µg/g for Al; 30.0–81.0 µg/g for Ca; 11.9–60.4 µg/gfor Cl; 1.43–5.96 µg/g for Cu; 7.3–28.1 µg/g for Mg;0.47–1.69 µg/g for Mn; 17.5–72.8 µg/g for Na and 0.04–0.07µg/g for V. The experimental procedure is suitable for routine determinationof micronutrient element in foods for control and monitoring purposes.     

The determination of eear elements in aircraft engine oil filter debris by neutron activation analysis

The increasing trend towards the use of fine oil filtration in modern jet engines suggests that the Spectrometric Oil Analysis Program (SOAP), which routinely monitors the health of aeroengines, may no longer be effective in detecting abnormal wear trends. Since the oil filter contains a wealth of information on wear in a system, it may be necessary to perform engine health monitoring through Filter Debris Analysis (FDA). In the present study, a method was developed for the determination of 19 wear elements (Ag, Al, Au, Cd, Co, Cr, Cu, In, Fe, Mg, Mn, Mo, Ni, Sb, Sn, Ti, V, W and Zn) in aircraft engine oil filter debris samples using the analytical technique of Neutron Activation Analysis (NAA). Results obtained by NAA for the analysis of two types of filter debris samples compared well with results obtained previously for similar samples and it appears that FDA should be very useful for following wear trends.     

The determination of bromine in rocks by neutron activation analysis

A neutron activation method for the determination of bromine in rocks and minerals is described. After removal of iodine, bromine is separated by oxidation with potassium permanganate and extraction with carbon tetrachloride. Bromine is thon precipitated as silver bromide; yields are from 60 to 84%. The method has a sensitivity of 0.001 p.p.m. of bromine and is free from interfering reactions. The values obtained for G-1 and W-1, 0.484 and 0.490 p.p.m. of bromine respectively, are lower than the average values for granites and basalts previously reported.     

The determination of sampling constants by neutron activation analysis

It has been found that sampling constants vary greatly not only from major elements to trace elements, but also between individual trace elements. A comprehensive investigation of a potential reference material therefore requires the determination of sampling constants for all elements to be certified, and other analytical methods therefore have to be included. For methods in statistical control the described strategy can be applied.     

Indirect determination of soluble trace elements in certified reference materials by neutron activation analysis

Since 1983 we have analyzedaqua regia extracts from environmental reference materials of 5 different soils and 4 different sludges by neutron activation analysis. Aqua regia as such is not accepted for irradiation in a nuclear reactor, and therefore the solution has to be evaporated to dryness, mixed and dried to constant weight before an aliquot can be taken and subjected to instrumental neutron activation analysis (INAA). Results for leachable Cr and Zn were found to display greater variability than results for total contents of these elements, and the reasons for this will be discussed.For the 1994 certification campaign for one soil and two sludges we have chosen to determine the total content of trace elements in these reference materials by INAA before and afteraqua regia leaching. The leachable contents are then found indirectly as a difference between the two results; in this way we eliminate the sources of uncertainty associated with the drying and handling of theaqua regia extracts, and we reduce the contributions from counting statistics.     

The determination of trace elements in new food grain SRM's using neutron activation analysis

Potentially toxic metals in the food chain that can lead to deleterious effects on human health have been well documented. Because of the toxicity of some metals, levels of 1 ppm or less must be routinely monitored in foods to ensure human safety. To ensure the accuracy of measurement, NBS in a cooperative interagency agreement with the Food and Drug Administration is involved in developing and certifying selected elements in food grain as a part of the Standard Reference Material program. Both instrumental and radiochemical neutron activation analysis were used to analyze two food grain standard reference materials (Rice and Wheat Flours) for trace element certification.     

Multielement-standards for determination of trace elements in water by neutron activation

Summary For the determination of trace elements in water by neutron activation (NAA) two multielement-standards on the basis of calcium carbonate were prepared by freeze-drying from solutions after addition of calcium carbonate. Homogeneity was certified by NAA, and the content was tested by atomic absorption (AAS), NAA and X-ray fluorescence analysis (XFA). The multielement-standards were applied for trace element determination in standardized water samples and in Rhine water. Comparison with a monoelement-standard (iron) and with AAS showed good agreement of the results.

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Multielement-Standards für die Bestimmung von Spurenelementen in Wasser durch Neutronenaktivierung

Zusammenfassung Zwei Multielement-Standards auf Basis von Calciumcarbonat wurden durch Gefriertrocknung von Lösungen nach Zusatz von CaCO₃ hergestellt. Die Homogenität wurde durch NAA bewiesen und der Gehalt durch AAS, NAA und Röntgenfluorescenz geprüft. Die Standards wurden für die Spurenelementbestimmung in standardisierten Wasserproben und in Rheinwasser angewendet. Vergleiche mit einem Monoelement-Standard (Eisen) und der AAS zeigten gute Übereinstimmung der Ergebnisse.

     

The determination of trace metals in lubricating oils by atomic spectrometry

The determination of trace metals in lubricating oils using atomic spectrometric methods is reviewed. The importance of such analyses for technical diagnostics as well as the specific sample characteristics related to the analyte form (metallo-organic and metal particles) is discussed. Problems related to sample pre-treatment for appropriate sample introduction and calibration are addressed as well as the strategies to overcome them. Recent trends aimed at simplifying sample manipulation are presented. The applications and scope of AAS, ICP OES and ICP MS techniques for the determination of trace metals in lubricating oil is individually discussed, as well as some present instrumental trends.     

Multielemental determination in water by neutron activation analysis

Instrumental neutron activation analysis (INAA) technique has been applied to a water sample to determine the elemental concentrations. The sample was irradiated at a neutron flux of 1.2·10¹² n·cm^–2·s^–1 for two different periods followed by counting at three different decay times, using two coaxial type high-resolution Ge(Li) detectors. The dominant elements detected in the water sample are Ca, Cl, Na, Mg, and K present in levels while Co, I, Mn, Sm, and Sb are present in smaller amounts approximately on the average 0.01 ppm. Only traces of other elements such as rare-earth elements, Ag, As, Ba, Cu, Cd, Fe, Sr, W, Zn, seem to be present in the water samples.     

Instrumental method for the determination of trace elements in water samples by neutron activation analysis

Thermal neutron activation analysis and a large-volume high-resolution Ge(Li) gammaray spectrometer, connected on-line to a DEC PDP 8/L computer, have been used to measure the concentrations of Na, Sc, Cr, Fe, Co, Ni, Zn, As, Se, Br, Rb, Ag, Sb, Cs, W and Hg in some Italian subsurface water samples. The instrumental method requires neither a chemical separation technique nor a pre- or post-concentration of the trace elements to be detected. As a consequence, this method eliminates many inherent errors associated with chemical determinations. The technique is sensitive, precise and particularly suitable for routine analysis of many trace elements at both natural and pollution levels in water samples. The interferences due to fast neutron (n, p) and (n, α) reactions are not appreciable, with the only exception of the⁵⁴Fe(n, p)⁵⁴Mn and⁵⁸Ni(n, p)⁵⁸Co reactions. Losses of volatile, elements, e. g. As, Br and Hg, during irradiation proved to be negligible.     

An optimum method for the determination of rare earth elements by neutron activation analysis

A scheme is described for the analysis of all 14 rare earth elements in rocks by neutron activation analysis using a group of radiochemical separation. The scheme takes particular account of the ‘difficult’ rare earth elements and is designed to minimise both γ-spectrometer counting time and overall analysis time.     

Multi-element analysis of Ghanaian crude oils by instrumental neutron activation analysis

Instrumental neutron activation analysis based on thermal neutrons from the Ghana Research Reactor-1 facility was utilized to analyze 18 trace elements namely Al, As, Br, Ca, Cd, Cl, Co, Cu, Fe, K, Mg, Mn, Na, Ni, S, Si, V, and Zn in two different crude oil samples from the Saltpond and Jubilee field in the Saltpond, Central region and Cape Three Points, Western region of Ghana, respectively. The sulfur concentration for both samples were low and within globally accepted range of 0.1–0.5%wt for sweet crude oil. The results of the elemental analysis showed that the two samples are relatively low in trace element concentrations compared to crude oils of other countries. Higher Fe concentration in the Jubilee crude oil indicates younger oil. The V/Ni ratios obtained for crude oils from both locations imply a possible marine organic origin and also suggest the Saltpond crude oil is more matured than the Jubilee crude oil.     

The determination of nickel in air dust by neutron activation analysis

The determination of nickel in atmospheric aerosols, collected on filter paper, is performed by thermal neutron activation analysis using the⁶⁵Ni (T=2.56 h) isotope. Liquid-liquid extraction and anion-exchange are applied in the chemical separation. The absolute sensitivity of the method is ≌0.02 μg Ni. The relative sensitivity is 0.005 μg Ni/m³ if an air sample of about 1000 m³ is used.     

The determination of iodide in sea water by neutron activation analysis

A simple and sensitive method for the determination of iodide in sea water by neutron activation analysis has been developed. Iodide is separated from most other anions by passing sea water through a strongly basic anion-exchange column, recovered by elution with 2 M sodium nitrate, and concentrated from the eluate by precipitation as palladium(II) iodide in the presence of excess of palladium(II) with elemental palladium as carrier; elemental palladium is generated by reduction of some of the palladium(II) with thiosulfate. The precipitate is separated from the supernatant liquid by filtration. Checks on the efficiency of separation by means of added ¹²⁵I showed recoveries of 100 ± 3 %. The filter paper containing the precipitate is pressed into a pellet for neutron activation analysis by irradiation for 5 min at a flux of 4 ·10¹² n cm^?2 s^?1 and counting the ¹²⁸I 442.7-keV photopeak.