Mössbauer Study of El-Bahrain Meteorite

Procedures for the determination of traces of rare earth elements (REE) in geological samples by instrumental neutron activation analysis (INAA) and high resolution liquid chromatography (HPLC) are presented. The international standard reference materials AGV-1, GSP-1 and G-2 (USGS) were tested for the determination of REE concentrations using both techniques. The results obtained showed good agreement with certified values, giving relative errors less than 10%. By using INAA, the REE La, Ce, Nd, Sm, Eu, Tb, Yb and Lu were determined. All the REE, except Dy and Y, were determined when HPLC was employed. The application of INAA and HPLC to the determination of REE in geological samples is also discussed.     

Determination of 22 elements in geological samples by instrumental neutron activation analysis

An instrumental neutron activation analysis (INAA) method has been developed for multi-element determination in geological samples. The INAA method consists of irradiation of samples for 90 sec at a flux of 1.0·10¹² n·cm⁻²·sec⁻¹ and determination of 12 elements by using their short-lived nuclides. Samples have been re-irradiated for 3 hrs for measuring concentrations of another 10 elements. Precision and accuracy of the INAA method have been evaluated by analysing samples and USGS standard reference materials. Precision and accuracy are within±15% and ±10%, respectively.     

Effect of sample to detector geometry on the accuracy of instrumental neutron activation analysis and implications for the design of a simple automatic sample-changing wheel suitable for the routine counting of low activity geological samples

The effect of small geometric errors in positioning samples in front of gamma detectors during instrumental neutron activation analysis is discussed and it is shown that, for example, a 0.2 mm repositioning discrepancy for a source to detector distance of 10 mm can cause errors in measured activity of as much as 4 per cent. This calculation has been undertaken for a range of sample-detector distances (5–50 mm) in order to emphasise the importance of sample counting geometry on the accuracy of INAA calibrations. Criteria derived from this investigation have been used to design and construct a simple samplechanging wheel suitable for the routine analysis of low activity geological samples. The effect of the choice of sample wheel size on the magnitude of spectral interference between counting and non-counting samples mounted in the wheel has been considered.     

Determination of uranium fission interference factors for INAA

Instrumental neutron activation analysis (INAA) is a very suitable technique for the determination of several elements in different kinds of matrices. However, when the sample contains high uranium concentration this method presents interference problems of uranium fission products. The same radioisotopes used in INAA are formed in uranium fission. Among these radioisotopes are ¹⁴¹Ce, ¹⁴³Ce, ¹⁴⁰La, ⁹⁹Mo, ¹⁴⁷Nd, ¹⁵³Sm and ⁹⁵Zr. The purpose of this study was to evaluate uranium fission interference factors to be used in the INAA of environmental and geological samples containing high levels of U. The obtained interference factors agreed with literature reported values. The results point to the viability of using these experimentally determined interference factors for the correction of uranium fission products.     

A comparison of the capacity of FA-ICP-MS and FA-INAA

The platinum-group elements (PGEs) are commonly determined by INAA and ICP-MS after a NiS fire assay preconcentration. The results of the initial round robin for the PGEs and gold were examined for geological Canadian reference materials (WGB-1, TDB-1, UMT-1, WPR-1, WMG-1, and WMS-1). The Au accuracy is generally within 15% for both methods. For Ir, Os, Pd, Pt and Rh the accuracy for most samples is better than 10% for FA-ICP-MS and FA-INAA (true only for sulfide-bearing samples in the case of FA-INAA). Ru is not very accurate by either methods. Ru and Au have problems with precision which is interpreted to be related to the loss of gold in the dissolution step and for Ru, the source of the problem is not yet understood. Kurtosis show that FA-INAA has higher clustering than FA-ICP-MS for most analytes. It suggests a slightly better precision for FA-INAA. This is explained by the robustness of INAA after the NiS preconcentration despite its lower instrumental precision versus the complex dissolution steps involved in ICP-MS. For samples richer in PGEs (sulfide- and/or oxide-bearing rocks) both methods perform adequately but for low PGEs concentration samples (crustal rocks) ICP-MS shows an advantage.     

Speciation of the inorganic components in brown coal

Brown coal samples from different deposits have been analyzed for the bonding forms of their inorganic components. Besides the analysis of the dried coals, ashing techniques (high and low temperature ashing) and extraction procedures with different solvents (acids, bases, complexation agents, organic solvents with different polarity) have also been investigated. ESCA, PIXE, INAA, ICP-Atomic Emission Spectroscopy, NMR and Ionchromatography have been applied to the analysis of coals, ashes, wet ashing and extraction products. The bonding behavior of more than 40 elements could be characterized. Conclusions about geological and geochemical processes during and after coalification could be drawn.     

Gold-Silver Mineralization in Submarine Hydrothermal Sulphides: INAA Results After Ten Years of Intense Prospecting

During the last twenty years, IFREMER has organized many diving cruises to collect geological, mineralogical and geochemical data on submarine hydrothermal mineralization. Gold and chalcophile trace elements have been determined by instrumental neutron activation analysis (INAA) in Pierre Süe Laboratory. Particularly for gold and silver determination, but also for In, As, Sb, Se, INAA is the most sensitive instrumental procedure. Typically, the East-Pacific Rise (EPR) deposits are gold-poor compared with the Mid-Atlantic Ridge (MAR) and the Lau Basin deposits. Our INAA data plotted in a Au-Ag diagram support the difference between back-are basin mineralization and spreading oceanic ridges. The most interesting samples for gold prospecting have been discovered in the Logatchev hydrothermal field at 14°45 N on the Mid-Atlantic Ridge: they show an exceptionally high mean content of gold, about 9 ppm, with a maximum of 56 ppm for one sample which contains significant amounts of native gold and electrum. It is the first conclusive evidence of a primary gold-copper association in seafloor sulphides. This may be compared with fossil hydrothermal deposits from the Oman ophiolitic complex.     

Use of geologically biased enrichment factors (EF) as indicators of natural air pollutants

Airborne samples representing dustfall, street, and household dusts of Aswan were collected; and ten elements (Si, Ti, Fe, Mn, K, Al, Ca, Mg, Na, and P) were chemically analysed by means of instrumental activation analysis (INAA), inductively coupled plasma (ICP), and X-ray fluorescence (XRF). The puzziling differences in the values of the enrichment factors (EF) and obvious contradiction with the mineralogy of the dustfall samples both indicate that this method of calculation could help to establish models of dust matrices in different geological and industrial regions rather than considering it only as a tool for assessing the source rocks.     

A comparison of INAA and ICP-MS/ICP-AES methods for the analysis of meteorite samples

Instrumental neutron activation analysis (INAA), inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP mass spectrometry (ICP-MS) (hereafter, ICPs) were applied to meteorite samples for the determination of elemental content. The analytical applicability and suitability of the three methods have been compared. Those comparisons led to the refinement of our analytical procedures for INAA and ICPs, yielding more reliable data. Our INAA data proved to be reliable enough for classifying meteorites, while the ICPs, especially ICP-MS, can characterize elemental abundance features in detail, as demonstrated by REE abundance patterns for the Allende meteorite. In this manner, INAA and ICPs can be used in a complementary fashion in cosmochemical studies.     

Analytical procedure for the determination of thorium, zinc and potassium in diet samples

Instrumental neutron activation analysis (INAA), and atomic absorption spectrometry (AAS) have been used for the determination of trace amounts of thorium, zinc, and potassium in diet samples. Interlaboratory comparison has been made. The z-scores show that INAA can be used to determine thorium and zinc whereas AAS can be employed to determine potassium in diet samples.     

Determination of Sodium in Magnesian and Aluminiferous Materials by INAA using a Thermal Column

Several ppm of sodium can be determined in aluminum, alumina and magnesia samples by INAA in which fast neutron interferences are corrected by irradiating the samples in various locations of the thermal column different in fast to thermal neutron flux ratio. A simple INAA using thermal column is effective for sodium determination in geochemical standard reference samples of peridotite and dolomite containing considerable amount of magnesia as one of the matrix elements.     

Neutron activation analysis of the rare earth elements in rocks from the earth's upper mantle and deep crust

Three techniques for analyzing rare earth elements (REE) in geological materials are described, i.e. instrumental neutron activation analysis (INAA), neutron activation analysis with pre-irradiation chemical REE separation (PCS-NAA) and radiochemical neutron activation analysis (RNAA). The knowledge of REE concentrations in eclogites, peridotites and minerals from the earth's lower crust and upper mantle is very useful in constraining their petrogenetic history.     

Investigate the capability of INAA absolute method to determine the concentrations of 238U and 232Th in rock samples

This work aimed to study the capability of INAA absolute method in determining the elemental concentration of ²³⁸U and ²³²Th in the rock samples. The INAA absolute method was implemented in PUSPATI TRIGA Mark II research reactor, Malaysian Nuclear Agency (NM). The accuracy of INAA absolute method was performed by analyzing the IAEA certified reference material (CRM) Soil-7. The analytical results showed the deviations between experimental and certified values were mostly less than 10 % with Z-score in most cases less than 1. In general, the results of analysed CRM Soil-7 show a good agreement between certified and experimental results which mean that the INAA absolute method can be used accurately for elemental analysis of uranium and thorium in various types of samples. The concentration of ²³⁸U and ²³²Th ranged from 1.77 to 24.25 and 0.88 to 95.50 ppm respectively. The highest value of ²³⁸U and ²³²Th was recorded for granite rock sample G17 of ²³⁸U and sample G9 of ²³²Th, whereas the lower value was 1.77 ppm of ²³⁸U recorded in sandstone rock and 0.88 ppm of ²³²Th for gabbro. Moreover, a comparison of the ²³⁸U and ²³²Th results obtained by the INAA absolute method shows an acceptable level of consistency with those obtained by the INAA relative method.     

Speciation and instrumental neutron activation analysis for arsenic in water samples

Ground water samples obtained from West Bengal, India were analyzed for total arsenic and its inorganic species contents by instrumental neutron activation analysis (INAA). Two anion exchange separation methods using Dowex 1X8 in chloride and acetate forms were standardized for the speciation of As(III) and As(V) using radiotracers. The method by Dowex 1X8 in the acetate form was validated using synthetic mixtures of As(III) and As(V), and applied to water samples; the species concentrations were determined by INAA. The accuracy of the INAA method was evaluated by analyzing the NRCC CRM DORM-2 for total arsenic.     

Multielement NAA for the characterization of Saudi Arabian rocks

The instrumental neutron activation analysis technique (INAA) was used in the qualitative and quantitative analysis of 48 geological samples from the Umm Al-Birak area in the Kingdom of Saudi Arabia. The samples were properly prepared together with their standards and simultaneously irradiated in a neutron flux of 2.4 ·10¹² n·cm^–2 s^–1 in the reactor facilities of the National Tsing Hua University (THOR) in Taiwan. Gamma-spectra from the high resolution Ge(Li) detector were analyzed using the BRUTAl code. As a result of the analysis of the geological samples, 20 trace elements were identified qualitatively and quantitatively. These elements are: Co, Cr, Eu, Fe, Hf, K, La, Lu, Na, Rb, Sc, Sm, Ta, Tb, Th, U, Yb, Zn and Zr. The concentrations of these elements have been used in the investigations of the geochemistry of the Umm Al-Birak microgranite site using the BMDP computer code of the Ministry of Petroleum and Mineral Resources. This investigation showed that the high grade area is a differentiated rock that crystallized in a late stage of the Umm Al-Birak microgranite area.     

The use of Big Sample INAA for inhomogeneous materials: Homogenizations no longer needed?

Two samples of one litre each of mercury contaminated soil were analyzed by Big Sample INAA. Using this method, sample preparation procedures can be omitted and the number of sample size reduction steps are decreased. Therefore, the representativity of the sample is improved. Afterwards, Big Sample INAA is compared to standard INAA by analyzing ten subsamples taken from each one litre sample. It is concluded that multi-element analysis results of Big Sample INAA are valid even for inhomogeneous large samples. This paper presents the first concentrations measured with BSINAA.     

Analytical data of geologic obsidians from Japan by INAA using middle- and long-lived nuclides

This paper reports the results of instrumental neutron activation analysis (INAA) on 3,704 obsidian samples, taking the measurements of 23 elements. The results are summarized, combining the results of INAA conducted earlier by Ambiru et al. on 1,444 samples. The samples for these analyses are taken from seventy obsidian sources located at various places of Japan.     

Geological reference materials for standardization and quality assurance of instrumental neutron activation analysis

Results are presented from the INAA of 34 elements in NIST and USGS geological reference materials that were analysed relative to multielemental SRM-1633a Coal Flyash standards. The data compare favorably with works reported by other investigators. The application of historical control charts for continuous monitoring of quality assurance and detection of systematic errors is demonstrated.     

Comparison of the role of photon and neutron activation analyses for elemental characterization of geological,biological and environmental materials

The potential of photon activation analysis (PAA) for multielement trace analysis can hardly compare with that of neutron activation analysis (NAA). However, PAA appears superior over NAA for the determination of a number of elements, namely C, N, O, F, Mg, Si, Ca, Ti, Ni, Sr, Y, Zr, Nb, Sn, Tl and Pb in geological, environmental and biological materials. Most of these and other elements can be determined using nondestructive, instrumental PAA (IPAA), especially in geological materials. The possibilities of IPAA for multielement analysis using photoexitation and other photonuclear reactions are reviewed and compared with those of instrumental NAA (INAA), namely for geological materials. The need for and usefulness of radiochemical PAA (RPAA) procedures are also discussed.     

Marine gradients of halogens in moss studies by epithermal neutron activation analysis

INAA is known to be a powerful technique for the simultaneous determination of chlorine, bromine and iodine. In this paper INAA using epithermal neutrons is shown to be particularly useful to elucidate marine gradients of these elements. Examples are from a transect study in northern Norway where samples of the feather moss Hylocomium splendens were collected at distances of 0-300 km from the coastline. All three elements decrease exponentially as a function of distance from the ocean in the moss samples, strongly indicating that the atmospheric supply from the marine environment is the predominant source of these elements to the terrestrial ecosystem. It is suggested that environmental studies of halogens in general and iodine in particular is a promising future area of application for INAA, when employing epithermal neutrons. This revised version was published online in July 2006 with corrections to the Cover Date.