Routine multielement instrumental neutron activation analysis of silicate rocks using short-lived radionuclides

By means of thermal neutron activation and countings on the small planar and large coaxial Ge(Li) detector, 13 elements are determined in various silicate rocks, using short-lived radionuclides with half-lives from 2 min to 15 h. A method of routine analysis with simple dead-time and pile-up correction is described and tested with the standard rocks AGV-1 and G-2.     

Fast neutron activation analysis using short-lived radionuclides

Fast neutron activation analysis experiments were performed to investigate the analytical possibilities and prospective utilization of short-lived activation products. A rapid pneumatic transfer system for use with neutron generators has been installed and applied for detecting radionuclides with a half-life from 300 ms to 20 s. The transport time for samples of total mass of 1–4 g is between 130 and 160 ms for pressurized air of 0.1–0.4 MPa. The reproducibility of transport times is less than 2%. The employed method of correcting time-dependent counting losses is based on the virtual pulse generator principle. The measuring equipment consists of CAMAC modules and a special gating circuit. Typical time distributions of counting losses are presented. The same 14 elements were studied by the conventional activation method (single irradiation and single counting) by both a typical pneumatic transport system (run time 3 s) and the fast pneumatic transport facility. Furthermore, the influence of the cyclic activation technique on the elemental sensitivities was investigated.     

Errors in instrumental neutron activation analysis

Equations are derived for the statistical and systematic error in INAA based on single photopeaks. They may serve to predict the applicability of the method or to judge data obtained under well-known conditions.     

Monostandard instrumental neutron activation analysis of Chinese Biological Standard Reference Material using short-lived radionuclides

A routine procedure for monostandard INAA using short-lived radionuclides with half-lives from 2 min to 15 hrs is described. Ten elements (Al, Mg, Ti, V, Mn, Cl, Na, K. Br and Cu) are determined in Chinese Biological Standard Reference Material (peach leaves). The quality of analysis was checked by analyzing the U. S. NBS Standard Reference Materials SRM-1571 and SRM-1648.     

Recent instrumental neutron activation analysis studies utilizing very short-lived activities

The advantages and disadvantages of utilizing very short-lived induced activities (half lives in the range of 0.3 sec to 60 sec) in neutron activation analysis are reviewed. Results obtained with the recently described fast-transfer system and deadtime correction system are presented. They include results for 12 elements (F, S, Cl, Sc, Ge, Se, Br, Y, Zr, Ba, W, Pb), in both steady-state and high-intensity pulse irradiations, in both unlined and cadmium-lined irradiation positions. The half lives of the 12 species studied range from 0.3 sec to 18.7 sec. Some further aspects of the deadtime correction system are discussed.     

Beta spectroscopy of short-lived radionuclides using in-cocktail neutron activation

Low-flux, in-cocktail neutron activation analysis was used to quantify atmospheric tracer aerosols. Liquid scintillation was necessary to reduce the experimental uncertainty due to low sample activity. Activation of the tracers was performed in-cocktail since the short half lives of the nuclides did not allow time for sample preparation. Most of the tested cocktails proved inadequate for such analysis because of activation of their components. Neutron and gamma induced luminescence, and neutron generated bubbles in suspensions introduced further difficulties. Only a few cocktails showed activity levels after irradiation comparable to background. This method allowed substantial cost reduction by eliminating the need for irradiation in a research reactor.     

A software counting loss correction method for neutron activation analysis with short-lived radionuclides

A method has been developed for the correction of counting losses in NAA for the case of a mixture of short-lived radionuclides. It is applicable to systems with Ge detectors and Wilkinson or successive approximation ADC's and will correct losses from pulse pileup and ADC dead time up to 90%. The losses are modeled as a constant plus time-dependent terms expressed as a fourth order polynomial function of the count rates of the short-lived radionuclides. The correction factors are calculated iteratively using the peak areas of the short-lived radionuclides in the spectrum and the average losses as given by the difference between the live time and true time clocks of the MCA. To calibrate the system a measurement is performed for each short-lived nuclide. In a test where the dead time varied from 70% at the start of the measurement to 13% at the end, the measured activities were corrected with an accuracy of 1%.     

Cumulative neutron activation of short-lived radionuclides for the analysis of large samples in mineral exploration

Cumulative neutron activation is used to determine mg/kg concentrations of gold in rock samples, weighing 10 g. Twenty 0.5 g replicates are irradiated in an epithermal-neutron flux for 5 s and counted for 14 s. The twenty spectra are summed, and gold is measured with the 279 keV gamma-ray of^197mAu (7.2 s). Total analysis time for a 10 g sample is 400 s and detection limits around 2 mg/kg are achieved in gold ores, sulfides and silicates.     

Erros in instrumental neutron activation analysis

Equations are derived for the statistical and systematic error in INAA. It is possible to use them for the definition of limits of decision, detection and determination.     

Anticoincidence counting further improves detection limits of short-lived products by pseudo-cyclic instrumental neutron activation analysis

A systematic investigation was carried out on the merits and limitations of anticoincidence counting for short-lived radionuclides (t _1/2 < 75 s) used in instrumental neutron activation analysis (INAA) and pseudo-cyclic INAA (PC-INAA) methods for single as well as simultaneous multielement determinations in botanical and nutritional reference materials. The list of radionuclides of interest included: ¹⁰⁸Ag, ¹¹⁰Ag, ^165mDy, ²⁰F, ^75mGe, ^179mHf, ^86mRb, ^46mSc, ^77mSe, and ^177mYb. Precision and accuracy of measurements were good, and detection limits were of the order of µg kg^?1.     

Monitoring of neutron flux changes in short-lived neutron activation analysis

It is well known variations in neutron fluxes can adversely affect the final result in neutron activation analysis. The monitoring of neutron flux changes are usually described for medium and long-lived NAA using foils of cobalt, gold, zirconium, etc. However, for short-lived neutron activation analysis there appears to be no systematic study of the variations of the neutron flux. With our new automatic pneumatic system, where irradiation timing, decay and counting and position are very reproducible, we have performed a series of experiments using thermal and epithermal neutrons using aluminum wire as a monitor to monitor the neutron fluxes. Our experiments confirm that neutron flux fluctuations in the worst case can be up to ±12 % with a SD of 2–3 %. This effect can be seen regardless of the irradiation time and must be taken into consideration to achieve the best result.     

Evaluation of boron for the epithermal neutron activation analysis of short-lived radionuclides in geological and biological matrices

The value of boron, in addition to cadmium, as a thermal neutron filter for the epithermal neutron activation of short-lived radionuclides is shown to depend on sample matrix. Activation ratios of fifty nuclides are measured and the improvement in sensitivity is calculated for geological and biological matrices. The addition of boron, in the case of geological samples where the major interference is Al, improved detection for only F, Y, Sn, Ba, Er, W and Pt. In biological samples where Na is a problem the detection limits for F, Br, Rb, Y, Mo, Pd, Sn, Sb, I, Ba, Nd, Sm, Gd, Er, Hf, W, Re, Pt, Au, Th and U are all theoretically improved.     

14 MeV neutron activation analysis using short-lived products

Cyclic activation using pneumatic shuttling system and switch off and on the neutron source and detector are described in order to eliminate some uncertainties by the provision of more accurate timing, the measurement of the effective activating neutron flux and the correction for the detection system dead time.     

New perspectives for very short-lived neutron activation analysis

Recent attempts to improve the performance of very short-lived neutron activation analysis are reviewed. It is shown that the combination of an intense cold neutron beam from a research reactor with a beam chopper offers higher signal-to-background ratio, more accurate timing and much simpler sample handling than conventional cyclic activation analysis. Application of a digital spectrum analyzer in data list mode allows for easy determination of the half-life. Hence, time-resolved activation analysis utilizing energy and time information becomes practical. This revised version was published online in July 2006 with corrections to the Cover Date.     

Industrial applications of instrumental neutron activation analysis

Neutron activation analysis is shown as a useful diagnostic technique in semiconductor industry. A better acceptance of the method for applications in industry has been achieved through a specialized analytical service. Its main application is the characterization of high purity silicon in all stages of production. Irradiation of large sample volumes allowes a very sensitive detection of impurities in silicon with detection limits down to 10^–16 g/g. Other applications discussed are the analysis of silicon carbide, quartz, pure water and titanium. Special techniques described are autoradiography, depth profiling and surface analysis. In semiconductor process technology NAA was used to monitor contamination of silicon wafers.     

Precision high-speed neutron activation analysis via very short-lived activities

An automated, highly reproducible fast-transfer system (0.36±0.01 sec) has been developed, an oscillator/multichannel-scaling system has been developed to follow rapidly-changing spectrometer dead-times, the mathematics has been developed, and the data processing steps have been computerized. Three induced activities have been studied in some detail:^207mPb (0.80 sec),^38mCl (0.70 sec) and²⁰F (11.03 sec). Both steady-state and high-intensity pulsed reactor irradiations, with and without a Cd liner, have been used. The dead-time correction method has been carefully checked, and the overall method has been tested by the analysis of two NBS Standard Reference Materials: orchard leaves (for Cl and Pb) and bovine liver (for Cl). This paper represents a portion of the Ph. D. thesis of D. A. MILLER.     

Instrumental neutron activation analysis technique using subsecond radionuclides

The fast irradiation facility Mach-1 installed at the Danish DR 3 reactor has been used in boron determinations by means of Instrumental Neutron Activation Analysis using¹²B with 20-ms half-life. The performance characteristics of the system are presented and boron determinations of NBS standard reference materials as well as fertilizer materials are compared by literature value and spectrophotometric measurements, respectively. In both cases good agreement is obtained.     

Multielement analysis of lichen by instrumental neutron activation analysis

Lichen (species Trypethelium Eluteriae) is analysed for different elements. Nondestructive instrumental neutron activation analysis is employed for the multielemental analysis. Gamma-ray spectrometry is used for the identification and quantitative estimation of elements. Concentrations of 24 elements are reported. Gamma-ray spectrum of the lichen irradiated for 16 hours, delayed for 10 days, and counted for 10 hours on a 50 cm³ coaxial Ge(Li) detector is given.     

Elemental analysis of limestone by instrumental neutron activation analysis

Limestone samples from Assuit Governrate in Upper Egypt were subjected to elemental analysis by instrumental neutron activation analysis and X-ray fluorescence techniques. The samples were properly prepared together with their standards and simultaneously irradiated in a neutron flux of the order 7 × 1011 n/cm² s using TRIGA research reactor at Mainz. After activation the samples were subjected to γ-ray spectrometry using a high purity germanium detection system and computerized multichannel analyzer. Nineteen elements: Na, Ca, Mn, Fe, Sc, Cr, Co, Zn, Sn, La, Ce, Nd, Eu, Sm, Yb, Lu, Hf, Th and U were analyzed. X-ray fluorescence spectrometry have been also used. The presence of any elements in higher or lower levels in certain limestone samples is contingent on the occurrence of its bearing minerals, nature of parent sediments and depositional environments of these sediments. The major elements in the samples were also observed to be among the elements that had high enrichment factors in the study of suspended dust particulate within and around cement industries. This confirms cement as the major contributor to the airborne particulate matter in the environs.     

Epithermal neutron activation analysis of short-lived nuclides in geological material

The cadmium ratios of 52 short-lived nuclides have been measured. Epithermal neutron irradiation reduces the activities of²⁰F,²⁷Mg,²⁸Al,³⁸Cl,⁴⁹Ca,^46mSc,⁵¹Ti,⁵⁶Mn and⁶⁶Cu by factors of 20–30. The calculated improvements in detection limits for Ga, Br, Rb, Y, Mo, Rh, Pd, Ag, In, Sn, Sb, I, Ba, Nd, Sm, Gd, Dy, Er, Yb, Hf, W, Re, Pt, Au, Th and U are in the range 1–6. Hafnium was measured in USGS rocks: AGV-1 (4.9 μg g⁻¹), G-2 (7.5 μg g⁻¹) and GSP-1 (14.7 μg g⁻¹) and IAEA standards: SOIL-5 (6.3 μg g⁻¹ and SL-1 (4.6 μg g⁻¹). CCRMP reference concentrates PTC and PTM were analysed for rhodium (1.1 and 0.75 μg g⁻¹, respectively) and silver (69 and 5.8 μg g⁻¹, respectively).