Neutron activation analysis of low level lithium in water samples

For determining low level lithium concentrations in water, a neutron activation method based on the measurement of tritium radioactivity produced by⁶Li(n,)³H reaction has been developed. This method is specific and free from interference by other chemical elements. Using a low background liquid scintillation counter for tritium measurement, the detection limit is approximately 0.3 ppm during irradiation at a thermal neutron flux density of 1.1·10⁷n·cm^–2·s^–1 for 6 hours by a small nuclear reactor and liquid scintillation counting for 2000 minutes     

Quantification of estrogenic mycotoxins at the ng/L level in aqueous environmental samples using deuterated internal standards

Because of their pronounced estrogenicity, resorcyclic acid lactones (RALs) are of concern in aqueous environments even at the low ng/L level. Therefore, we developed an accurate, precise and sensitive HPLC-MS/MS method to detect these mycotoxins in different aqueous environmental samples. The compounds investigated included zearalenone (ZON), alpha- and beta-zearalenol, zearalanone as well as alpha- and beta-zearalanol. The use of isotope labelled internal standards (in this case deuterated RAL-analogues) ensured an accurate quantification of the target analytes, independent of matrix compounds interfering with the analytes during ionisation and analyte losses occurring during sample preparation. Sample enrichment was carried out by solid-phase extraction (SPE) using Supelclean Envi-18 cartridges. Absolute method recoveries for all analytes ranged from 95 to 108%, 70 to 102%, and 76 to 109%, method detection limits from 0.5 to 2.1 ng/L, 0.4 to 1.1 ng/L, and 0.8 to 12.4 ng/L and precision from 3 to 14%, 2 to 13% and 4 to 16% in drainage water, river water and wastewater treatment plant (WWTP) effluent, respectively. The method was applied to verify the emission of RALs from a Fusarium graminearum infested crop field into the drainage system. Zearalenone was present in drainage water in concentrations up to 30 ng/L. So far, none of the other five investigated compounds have been detected.     

Activation analysis for mercury in biological samples at nanogram level

A new method has been devised for determining mercury in samples of biological origin. It is based on complete ignition of the sample in a silica tube, trapping volatile interfering activities such as bromine or chlorine, and selectively adsorbing mercury on a strip of filter paper which has been previously impregnated with elemental selenium. This strip is later counted for quantitative evaluation. The versatility of the method has been demonstrated by the analysis of a wide range of samples such as water, cellulose, flour, fish solubles or animal blood samples with mercury contents between 1 and 200 ng g of sample.     

Deuteron activation analysis of geological samples

Deuteron activation was found to be suitable for analysing geological samples, as no interfering activities are formed from oxygen, silicon and aluminium, which together make up more than 80% by weight of the earth's crust. To test the applicability of this method to geological samples, the mineral tourmaline was activated with 5.5 MeV deuterons obtained from the 6 MV van de Graaff accelerator at the Southern Universities Nuclear Institute. The induced activities were measured and analysed by gammaray spectrometry and the elements Al, Mg, B, Mn, Na, Fe and Li could readily be determined.     

Epithermal neutron activation analysis and detection limit calculation for trace amounts of thorium at nanogram level,in Israeli geological samples

Trace amounts of thorium in Israeli geological samples were determined by epithermal neutron activation analysis followed by high resolution gamma-ray spectrometry. Epithermal neutron irradiation has the advantage of enhancing the production of²³³Th via the²³²Th _→ ^{n,γ 233}Th reaction over that of interfering nuclides which have a lower I_o/σ_o ratio. The delay time between the end of irradiation and the start of measurements was shortened to 1–2 days. Under the experimental conditions described, the detection limit of Th was 3.3±0.7 ng. The method is nondestructive, accurate and highly sensitive.     

A simple method for determining ammonia in water at the ppm level

Summary A simple colorimetric method is described for the determination of ammonia in water at the ppm level. Indophenol blue color is produced in an alkaline borate medium using phenol and hypo-chlorite as reagents. Comparison of color intensity is carried out by means of test tubes. When metal ions that interfere with ammonia determination are present in water, the interference can be prevented by applying a diffusion technique.

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Zusammenfassung Eine einfache kolorimetrische Methode zur Bestimmung von ppm-Mengen Ammoniak in Wasser wurde beschrieben. In Alkaliborat-Medium führen Phenol und Hypochlorit als Reagenzien zur Bildung von Indophenolblau. Der Farbvergleich wird in Reagensgläsern durchgeführt. Befinden sich im Wasser störende Metallionen, so kann man diese Störung mit Hilfe der Diffusionstechnik umgehen.

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Visiting professor at the University of Singapore, 1975–1976, on sabbatical leave from the City University of New York.     

Novel Helmholtz-based photoacoustic sensor for trace gas detection at ppm level using GaInAsSb/GaAlAsSb DFB lasers

A new and compact photoacoustic sensor for trace gas detection in the 2-2.5 microm atmospheric window is reported. Both the development of antimonide-based DFB lasers with singlemode emission in this spectral range and a novel design of photoacoustic cell adapted to the characteristics of these lasers are discussed. The laser fabrication was made in two steps. The structure was firstly grown by molecular beam epitaxy then a metallic DFB grating was processed. The photoacoustic cell is based on a Helmholtz resonator that was designed in order to fully benefit from the highly divergent emission of the antimonide laser. An optimized modulation scheme based on wavelength modulation of the laser source combined with second harmonic detection has been implemented for efficient suppression of wall noise. Using a 2211 nm laser, sub-ppm detection limit has been demonstrated for ammonia.     

241Am-XRF analysis of rare earths in geological samples

Rare earths in sediments are analyzed by X-ray fluorescence using²⁴¹Am as an excitation source. The analytical sensitivity lies in the ppm range.     

Target preparation of biological samples for trace element analysis using nuclear techniques

An easy and rapid method for preparing biological targets for trace element analysis using nuclear techniques involving charged particle beams is described. The targets are thin, homogeneous and uniform. They withstand 100 nA of 1–2 MeV proton beams and of 5–10 MeV alpha beams for about 10 hrs.     

Determination of fluorine in geological samples using accelerator derived neutrons

A fast, neutron activation analysis technique is described for the determination of fluorine in geological samples. The method utilises the reaction¹⁹F(n,α)¹⁶N for the determination. However, it avoids the interference reaction from oxygen which produces the same radionuclide since the neutrons are derived from the bombardment of beryllium with 3 MeV deuterons. The maximum energy of the neutrons so produced is well below the threshold for the competing oxygen reaction. The results indicate that the method gives acceptable accuracy over the range of a few tens ppm to several percent fluorine content using suitable standards. Sample analysis time is only a few minutes allowing the analyses of large numbers of samples per day.     

Detection of geological faults using a nuclear method

It proved possible to detect the precise location of large geological faults using the amount of⁴⁰K and²²⁰Rn daughter gamma-rays and the amount of²²²Rn (measured in a scintillation chamber) which could be extracted from the soil using negative pressure. Both⁴⁰K and²²⁸Th appear to be concentrated in fault gouge. The²²²Rn content extractable from the soil is a measure of permeability and is very low in the region of the fault due to clay-like fault gouge. The method was demonstrated successfully on the large Wellington fault at Upper Hutt, New Zealand.     

Instrumental neutron activation analysis of Moroccan geological samples using the k0-standardization method

Instrumental neutron activation analysis (INAA) for traces and major elements of several geological samples from “Zgounder” region in Morocco was performed utilizing the k ₀-standardization method. Sample irradiation has been done by the 250 kW Triga Mark II reactor at Jozef Stefan Institute in Slovenia. Due to its accuracy, sensitivity and specificity, the k ₀-standardization method is the most suitable method for non-destructive multielement analysis mainly for trace elements in rocks. It requires an accurate knowledge of the parameters of the irradiation facilities and other instrumentation parameters. It is an absolute standardization method, where the absolute nuclear data are replaced by a nuclear constant, the k ₀-factor, determined experimentally with high accuracy. More than 40 elements were determined using about 30-second short and about 7-hour long irradiations. Gamma-rays emitted from the irradiated samples have been determined by a high purity germanium detector. Accuracy was assessed using the standard reference material AGV-1. This was less than 1% for major elements and about 5% for traces. This revised version was published online in July 2006 with corrections to the Cover Date.     

Uranium analysis by K X-rays from geological samples

Uranium analysis at trace levels from geological samples was performed by K X-ray fluorescence using a semiconductor detector and radioisotope excitation. The exciting⁵⁷Co-source was constructed in such a way as to produce a high peak to background ratio. Using 10 minutes counting times the detection limit with a 0.26 GBq source was 24 μg/g improving to about 9 μg/g with a ten times stronger source. The detection limits for tin, cerium, tungsten and thorium were also measured.     

Light element profiling using nuclear reaction analysis on tapered corrosion sections

A scanned microbeam has been used to profile tapered corrosion sections of thickness up to 500 μm. The method of beam scanning and data collection is described and selected profiles are presented for the reactions D(³He, p)α,¹²C(d, p)¹³C,¹⁴N(p, α)¹²C and¹⁸O(p, α)¹⁵N. Finally the advantages and limitations of the technique are discussed.     

Low-blank digestion of geological samples for platinum-group element analysis using a modified Carius Tube design

We have developed a modified Carius Tube design that permits the low-blank digestion of geological samples prior to platinum-group element analysis. The new Carius Tubes incorporate a liner of high-purity quartz glass that retains the sample and acids during the digestion procedure. This dramatically reduces the comparatively high Pt blank associated with dissolutions in conventional Carius Tubes. Using the new Carius Tube design we are able to achieve total procedural blanks for the determination of the PGE in geological samples that are at the 1–15 pg/g level for Ru, Pd, Ir and Pt. This constitutes a reduction of blank values by a factor of ～10–100 compared to standard NiS fire assay sample preparation techniques.     

Low-blank digestion of geological samples for platinum-group element analysis using a modified Carius Tube design

We have developed a modified Carius Tube design that permits the low-blank digestion of geological samples prior to platinum-group element analysis. The new Carius Tubes incorporate a liner of high-purity quartz glass that retains the sample and acids during the digestion procedure. This dramatically reduces the comparatively high Pt blank associated with dissolutions in conventional Carius Tubes. Using the new Carius Tube design we are able to achieve total procedural blanks for the determination of the PGE in geological samples that are at the 1–15 pg/g level for Ru, Pd, Ir and Pt. This constitutes a reduction of blank values by a factor of ∼10–100 compared to standard NiS fire assay sample preparation techniques. Received: 23 September 1997 / Revised: 24 October 1997 / Accepted: 31 October 1997     

Neutron activation analysis of geological and biological samples using short-term reactor irradiation and successive counting

Short-term reactor irradiation followed by successive counting over long periods has been used for the nondestructive determination of more the 20 elements in geological and biological samples. The samples, along with USGS standards and NBS SRMs, were irradiated for 5 m, 10 m, 15 m, 1 h, 2.5 h, and 10 h, followed by counting on a Ge/Li/ gamma-ray spectrometer. The technique has been employed for the determination of several major, minor, and trace constituents in geological, biological and environmental samples.     

Measurements of Ir concentration in geological standard samples using neutron activation analysis with multiple gamma-ray coincidence method

In this study, the Ir concentrations in some standard rock samples were determined by using the multiple γ-ray detection method. The use of the multiple γ-ray detection method, which was developed for nuclide quantification, yielded better resolution and sensitivity than the ordinary singles γ-ray detection method. Iridium is one of the least abundant elements in Earth’s crust, with an average mass fraction of 0.001 ppm in a crust rock. However, iridium is relatively more abundant (concentration: 0.5 ppm or more) in undifferentiated meteorites. Therefore iridium abundance anomalies in geological samples provide important information about meteorite impact. The standard rock samples used in this study were SARM-76, FC-1 and FC-2. The SARM-76 was prepared from a platinum ore, and issued by the south African bureau of standards. FC-1 and FC-2 were obtained from fish clay sediment samples from Stevens Klint, Denmark.     

Analysis of geological samples by the micro-PIXE facility at KFUPM

Summary The scanning microprobe facility of the 3 MV Tandetron accelerator at King Fahd University of Petroleum and Minerals (KFUPM) has been applied extensively in various fields, including geology. This paper reviews a number of geological investigations carried out on samples of gold-bearing rocks, phosphorite ores and volcanic sediments. Elemental composition and distribution maps across single mineral grains, fluid inclusions, grain boundaries and matrices were measured. The microscopic data obtained are discussed to understand fundamental geological processes and ore genesis, and the provenance of economically important trace minerals contained in these samples.     

Determination of zinc in geological samples using Compton suppression with thermal and epithermal instrumental neutron activation analysis

The determination of Zn in geological samples using instrumental neutron activation analysis is usually done using the ⁶⁴Zn(n,γ)⁶⁵Zn reaction and its 244 day half-life. However this analysis has proven to be potentially difficult. This is due to its relatively low neutron absorption cross section and gamma ray intensity, and the relatively high neutron absorption cross section and gamma intensity of ⁴⁶Sc, which has an energy peak that is only 5 keV greater than ⁶⁵Zn. The use of a high resolution detector makes it possible to differentiate between the ⁶⁵Zn and ⁴⁶Sc photopeaks peaks. However, the dominating ⁴⁶Sc gamma ray can even make peak fitting routines unsuccessful in the proper determination of ⁶⁵Zn. The use of a Compton suppression system suppresses the ⁴⁶Sc peak, which has two coincident gamma-rays, and this greatly improves the ratio of the height of the ⁴⁶Sc 1120.5 keV photopeak to the ⁶⁵Zn 1115.4 keV photopeak. Irradiating the sample with epithermal neutrons also improves the measurement since ⁶⁵Zn has a higher cross section for epithermal neutrons rather than thermal neutrons, whereas ⁴⁶Sc has a higher thermal cross section. Another technique to determine zinc is the use of ⁶⁸Zn(n,γ)^69mZn reaction with its 13 h half-life using epithermal neutrons and Compton suppression INAA. However, the 438 keV gamma ray of ^69mZn has no interference with any adjoining photopeak. A critical comparison of these two methods is given.