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.     

A new approach to single-comparator instrumental neutron activation analysis

A new parametric approach to single-comparator instrumental neutron activation analysis (INAA) at the University of Missouri Research Reactor (MURR) was investigated. A detailed MCNP steady-state model of the MURR core was developed using the latest neutron data libraries to compute the continuous-energy neutron flux distribution. Intrinsic reaction rates were predicted by coupling the computed local flux distribution to the isotopic (n, γ) excitation functions for a range of elements present in standard reference materials (SRM). Using the predicted (n, γ) reaction-rates, the concentrations for the various elements were determined. The method worked well for all nuclides tested, including those with cross sections that are not proportional to 1/v such as Lu and Eu with agreements for most elements within 5% of the reference value.     

Decreasing the detection limits to ppq levels for high purity silicon analysis by instrumental neutron activation analysis with kilogram sampling weight

The amount of silicon sample used in instrumental neutron activation analysis (INAA) is generally less than twenty grams and the detection limits are in the range of ppb to ppt. The detection limits can be decreased further in several ways. Increasing neutron flux density, extending irradiation period and/or using more effective detector can improve the detection limits to some extent. Increasing sample weight, however, is a more feasible way to decrease the detection limits by a factor of hundreds with no new investment in existing irradiation/counting systems. In this work, two 8-inch high-purity silicon samples were analyzed by INAA to evaluate the validity and limitations of this concept in respect to neutron flux inhomogeneity, neutron shielding and -ray counting efficiency.     

Nuclear analytical techniques for quantification of uranium for its recovery from seawater

Nuclear analytical techniques namely fission track technique using solid state nuclear track detector (SSNTD) and instrumental neutron activation analysis (INAA) have been standardized and applied for quantification of low uranium concentrations in liquid samples such as feed, elute and brine and solid sorbent samples respectively. The quantification of uranium is required for its recovery study from seawater, which is one of the potential sources of uranium. The uranium concentration of a liquid sample obtained by SSNTD method was compared with the other well established conventional techniques like ICP-MS, ICP-AES, adsorptive stripping voltametry and alpha spectrometry. INAA was applied for uranium concentration determination in the radiation grafted polyamidoxime sorbent samples.     

The internal comparator method

An internal comparator method is proposed which offers reliable instrumental neutron activation analysis (INAA) results for samples with an irregular geometry and/or measured at the closest position to the Ge detector. Because the selected internal comparator in the sample analyzed will receive exactly the same thermal neutron flux as the other components, this method can be applied to the INAA of materials suffering from thermal neutron self-shielding. To apply the internal comparator method, the k₀-method must be installed and the analytes, including the internal comparator, should be homogeneously distributed in the test portion.     

Simultaneous determination of short-to-medium lived nuclides in Ghanaian food items using INAA and Compton suppression counting

Summary An instrumental neutron activation analysis (INAA) method was developed for the simultaneous determination of 19 elements in 10 individual food items from Ghana. The samples were irradiated for 1 minutes in a neutron flux of 2.5.     

Determination of vanadium in the presence of aluminium by neutron activation analysis

The precision of the determination of vanadium in the presence of aluminium by instrumental neutron activation analysis (INAA) was studied by varying the amount of aluminium in the sample. A precision of ±30% is obtained when the aluminium/vanadium ratio by weight is ∼350. When the ratio exceeds this value, it is probably desirble to perform a chemical separation prior to INAA in order to concentrate the vanadium content in the sample.     

BEAMGAA: A chance for high precision analysis of big samples

Summary In activation analysis of traces in small samples, the non-equivalence of the activating radiation doses of sample and calibration material gives rise to sometimes tolerable systematic errors. Conversely, analysis of major components usually demands high trueness and precision. To meet this, beam geometry activation analysis (BEAMGAA) procedures have been developed for instrumental photon (IPAA) and neutron activation analysis (INAA) in which the activating neutron/photon beam exhibits broad, flat-topped characteristics. This results in a very low lateral activating flux gradient compared to known radiation facilities, however, at significantly lower flux density. The axial flux gradient can be accounted for by a monitor-sample-monitor assembly. As a first approach, major components were determined in high purity substances as well as selenium in a cattle fodder additive.     

An automated neutron activation system for short-lived nuclides

The present paper describes an attempt to create a reliable and easy to use system for neutron activation with short-lived nuclides, suitable to be used with several irradiation and counting procedures in instrumental neutron activation analysis (INAA) at the Portuguese Research Reactor. This system can become very useful for a large community within LNETI, as well as other national institutes and universities, particularly for those involved in studies where the analysis of a large number of samples is required. Selenium determination has been performed, through the short-lived nuclide^77mSe, as an example of the reliability of the system.     

Chemical characterization of graphite by instrumental neutron activation analysis

Nuclear and commercial grade graphite samples were analysed by instrumental neutron activation analysis (INAA) using high flux reactor neutrons. Eleven elements (Na, K, As, Sc, Fe, Cr, Co, Zn, La, Ce, and Sm) were determined in eight samples of graphite (two nuclear grade and six commercial grade) by irradiating at a neutron flux of 3?×?10¹³ cm^?2 s^?1 in CIRUS reactor and assaying the activity by high-resolution gamma ray spectrometry using 40% relative efficiency HPGe detector coupled to an MCA. Concentrations of elements were determined by relative method of INAA. Results of both types of graphites as well as detection limits achieved by INAA method are discussed in the paper.     

A critical evaluation of short-lived and long-lived neutron activation products for trace element determinations

The application of short-lived nuclides in routine instrumental neutron activation analysis can reduce total experimental time per sample. The experimental sensitivities of short- and long-lived thermal neutron activation products of 32 elements are compared. The advantages of using short-lived nuclides are evaluated by comparing the precision, accuracy, and detection limits, using both short- and long-lived nuclides, for elemental determinations in biological, environmental and geological standard reference materials.     

Trace and major element compositions of Black Sea aerosol

Instrumental neutron activation analysis (INAA), flame atomic absorption spectrometry (FAAS), flame atomic emission spectrometry (FAES), graphite furnace atomic absorption spectrometry (GF-AAS), ion chromatography (IC) and visible spectrometry (VIS) were used to determine the composition of atmospheric aerosols, collected at a rural site in the Western Black Sea Coast of Turkey. A total of 354 daily aerosol samples were analyzed for 46 trace and major elements and ions. Sample preparation, quality control procedures, instrumental operating conditions for INAA and source apportionment work is presented.     

Optimal use of instrumental neutron and photon activation analyses for multielement determinations in sewage sludges

A combination of instrumental neutron activation analysis (INAA) and instrumental photon activation analysis (IPAA) methods has been developed for multielement determinations in a variety of sludges and fertilizers. The precision and accuracy of both the methods have been evaluated by analyzing replicate samples, NBS standard reference materials, and an interlaboratory intercomparison sewage sludge sample. The concentration rages of up to 50 elements in raw and chemical sludges, sludge-based fertilizers, and other organic and inorganic fertilizers are reported here. The advantages and limitations of the INAA and IPAA methods are also discussed here.     

Determination of gold in gold ores

The gold content of placer gold flakes and gold bearing ores has been determined by instrumental neutron activation analysis /INAA/ and radiochemical neutron activation analysis /RNAA/. It was discovered that significant errors result in the instrumental method for gold flakes as small as 10 mg due to sample self-absorption of neutrons during irradiation. Reliable results were obtained, for both ore samples and gold flakes, by dissolving the samples in aqua regia prior to irradiation.     

Metrological role of neutron activation analysis. IA. Inherent characteristics of relative INAA as a primary ratio method of measurement

In a series of three papers, the inherent characteristics of relative instrumental neutron activation analysis (INAA) as a primary ratio method of measurement, the unique functions of parametric INAA as an ideal back-up method of the relative INAA, and the valuable role of INAA in characterization of sampling behavior of individual elements in certified reference materials (CRMs) will be discussed. In this paper, the first of the series, the uncertainty evaluation and the traceability of values measured by neutron activation analysis (NAA), especially instrumental NAA (INAA), will be described to demonstrate the method at its ”the state-of-the-art” level can meet CCQM criteria for a primary ratio method. The scope and examples will be given. Received: 19 March 2001 Accepted: 2 October 2001     

Determination of thorium concentrations in soil and sand samples using instrumental neutron activation analysis

Thorium along with its daughter products present in the soil is one of the major contributors to the external gamma dose in the environment. To establish the dose levels, quantification of thorium contents in soil samples is very important. As a part of pre-operational environmental radiological surveillance, a total of 23 soil and six sand samples were collected from different locations around the proposed nuclear power plant site of Jaitapur, Maharashtra. Thorium concentrations in these samples were determined by instrumental neutron activation analysis (INAA). Samples were irradiated with neutrons in Apsara reactor at a neutron flux of?~5?×?10¹¹ cm^?2 s^?1 and radioactive assay was carried out using high resolution gamma ray spectrometry. Relative method of INAA was used for quantification of thorium utilizing 311.9?keV gamma ray of ²³³Pa, the daughter product of ²³³Th. The concentrations of thorium in the soil and sand samples were in the ranges of 4.0?C18.8 and 1.2?C6.2?mg?kg^?1 respectively.     

Sequential multielement analysis of a single aerosol filter by different instrumental and wet-chemical methods

Summary The direct instrumental methods X-ray fluorescence spectrometry (XRFS) and instrumental neutron activation analysis (INAA), and, after digestion of the sample, inductively coupled plasma mass spectrometry (ICP-MS) were applied in sequence to analyse small single aerosol filters. XRFS detected up to 19, INAA up to 22, and ICP-MS up to 33 elements. In total, up to 45 elements were determined, and, for a number of additional elements limits of detection could be given. For many elements, the data quality could be checked by cross-comparison of the results of two or all three methods. These methods very meaningfully complement each other and, in the manner used, allow the determination of all elements of interest in a small aerosol filter sample.     

New forms of the INAA advance prediction computer program

The development and experimental testing of a new instrumental neutron activation analysis (INAA) Advance Prediction Computer Program (APCP) is described for activation by high-intensity, short-duration reactor pulses. Also presented are the results of extensive experimental testing of the APCP for epithermal INAA. Brief mention is made of other forms of the APCP not yet completed, but in various stages of development.     

A study of environmental analysis of urban river sediments using activation analysis

Sediments of the Kitajukkengawa River (Sumida-ku, Tokyo, Japan) were analyzed by activation analyses. Concentrations of 36 elements for each sample were determined by instrumental neutron activation analysis (INAA) and neutron induced prompt gamma-ray analysis (PGA). Based on the correlation matrix between the elements in vertical distribution, principal component analysis (PCA) was performed. The degree of chemical weathering of silicate minerals was highest in the middle layer of the Kitajukkengawa River sediment and that adsorbed amount of trace metals such as Cd and Cr was increased along with chemical weathering.     

Optimized automated activation analysis

A combination of special techniques has been developed for optimization of experimental conditions in order to improve the analytical capability, to facilitate automation and to broaden the applicability of instrumental neutron activation analysis. The techniques used are: (1) compensation for the rapid radioactive decay of short-lived nuclides with the increase of the counting efficiency by automatic source movement to the detector during the counting period, to minimize count rate variations and to prolong the counting period, (2) repeated cyclic and cumulative activation to improve the counting statistics, (3) instrumental correction of counting losses at high and varying count rates by a loss-free counting system and (4) differentiation of the reactor neutron spectrum to enhance the counts from the nuclides of interest by reducing matrix interferences. By optimized combination and automation of these techniques significant improvement of the capability of instrumental neutron activation analysis can be achieved.