Instrumental neutron activation analysis of manganese,copper and vanadium in some commercial steel samples and of copper in copper base alloys

The instrumental neutron activation analysis (INAA) of industrially important steel samples, viz. IS-226, IS-2002, IS-2062, SS-304, SS-310, SS-316 and of copper base alloys, viz. high brass, gun metal and copper-silver alloys is carried out with a 2 Ci²⁵²Cf neutron source. The copper and vanadium content of all the steel samples and manganese content of former three steel samples are estimated by measuring the gamma activity of⁶⁶Cu,⁵²V and⁵⁶Mn radioisotopes, respectively, using a high purity germanium (HPGe) detector coupled to a 4 K multichannel analyzer (MCA). Similarly, the copper content of copper base alloys was also determined.Dedicated to Prof. H. J. Arnikar, Professor Emeritus, University of Poona, on the occasion of his 75th birthday.     

Instrumental neutron activation analysis of manganese in some industrially important steel samples

The manganese content of some industrially important steel samples viz. IS-226, spring steel, galvanized iron, high tensile steel, and mild steel is determined by instrumental neutron-activation analysis using a²⁵²Cf neutron source. The analysis is performed by measuring the activity of⁵⁶Mn after /n, / reaction on a 4 k multichannel analyzer coupled to a NaI/Tl/ detector at 847 keV, as well as on a single channel analyzer on integration mode coupled to a NaI/Tl/ detector. The results obtained by both procedures show reasonably good agreement with each other.     

Instrumental neutron activation analysis of tungsten in various steel samples

The instrumental neutron activation analysis /INAA/ of tungsten in various steel samples has been done with a 2 Ci²⁵²Cf fission neutron source having an integrated neutron flux of 10¹⁰ ns^–1 and measuring the -activity of¹⁸⁷W on a 4 K multi-channel analyzer /MCA/ coupled to a high purity germanium /HPGe/ detector. The tungsten content of various steel samples was between 0.017 and 0.024%.     

Simultaneous radiochemical determination of237Np and239Np with235Np as a tracer,and application to environmental samples

Neptunium is sorbed, together with plutonium, uranium and iron on Bio Rad AG 1×4 anion exchange resin from 9 mol/1 HCl, eluted with 7 mol/l HNO₃ and 1.2 mol/l HCl, purified on a second, identical column and electrodeposited on stainless steel discs.²³⁷Np is determined by -spectrometry,²³⁹Np by -spectrometry with a Ge detector, or via its 14.3 keV LX-rays in a Si(Li) measurement. The neptunium yield is determined from the count rate of the 13.6 keV LX rays of the tracer²³⁵Np in a later Si(Li) measurement. The average chemical yield is 78±11%. The detection limit for²³⁷Np is 1 mBq. The procedure allows the sequential determination of neptunium, together with plutonium, strontium, uranium and iron from one sample. The method was applied to air and total deposition samples from Munich-Neuherberg and to sediment samples from the Irish sea.     

Gamma-ray spectrometric analysis of neutron irradiated golden sands

A nondestructive method has been used for the qualitative and quantitative determination of elements such as Au, Cu, Ag in minerals and especially in golden sand. The induced radioactivity has been analyzed with a high resolution gamma spectrometer containing a Ge(Li) semiconductor detector type and a multichannel analyzer. The samples have been collected from the alluvia of the Mure and Someul Mic river basins, proving the presence of gold and copper in small concentrations. These results have been correlated to previous data showing the existence of some gold mines in these zones. This nondestructive, rapid and highly sensitive method can be used for industrial processes [1] control and prospections. The use of a NaI(Tl) scintillation crystal for routine measurements of the ¹⁹⁸Au radioisotope type and the interferences by copper, silver and indium in the irradiated samples are discussed.     

Gamma spectrometric analysis of ore samples from Sandur of Bellary, Karnataka, India

In the present paper the gamma spectrometric technique has been used to study the natural radioactivity levels present in the iron ore samples collected from the Sandur of Karnataka, India. This region, a member of Dharwar craton, known as Sandur schist belt is rich in Manganese and Hematite ore (Fe). The entire belt is characterized by numerous bands of banded magnetite and hematite quartzite. The ore samples were collected and prepared as per the ASTM standard procedures. The gamma spectrometric measurements were performed using a HPGe detector (Eurosys) based high-resolution 8k multi channel analyzer. The detector has a relative efficiency of 50% and resolution of 2.0?keV for 1.332?MeV gamma energy of ⁶⁰Co. The output of the detector was analyzed using a PC based 8k channel analyzer system. The mean activity concentrations of the ²³⁸U, ²³²Th and ⁴⁰K in the ore samples were found to be 14.59, 16.54 and 25.29?Bq/kg, respectively. The mean absorbed dose rate and the annual dose equivalent were estimated to be 18.97?nGy?h^?1 and 24.93???Sv?y^?1, respectively, which is lower than the world recommended average of 1?mSv?y^?1. The present work concludes that the natural radioactivity levels in ore samples of this region is within the natural limits and pose no health hazard to the public.     

Application of gamma-ray spectrometry for the assay of uranium in crude UF4—An input material used for producing nuclear grade U-metal at the natural uranium conversion plants

A -spectrometric method has been developed for the assay of uranium in crude UF₄, which is used as a secondary source of input material for producing nuclear grade U-metal at natural uranium conversion plants. The method makes use of a NaI (Tl) detector coupled with a multichannel analyzer. The 1 MeV -ray of²³⁸U is used for calibration. A method for the fabrication of uniform -assay calibration standards is also suggested, based on the results of this investigation. The calibration standards were prepared by soaking the matrix in uranium solution and then drying the whole material. The amount of²³⁸U in the crude UF₄ sample was directly estimated by comparing the areas under the 1 MeV -ray peak of known calibration standards with the corresponding areas of the samples to be measured. 100 g each of the standard and the sample were counted. 5 crude UF₄ samples were analyzed by this method. The uranium contents in these samples were found to be in the range of 12.2–28.7 g. To compare the -ray spectrometry results with a completely independent method, chemical analysis by potentiometry of all the samples was also done. The -spectrometric results were found to agree within ±18% with the chemical analysis results.     

Thermal neutron activation analysis of different varieties of mustard and sunflower seeds

Neutron activation analysis (NAA) technique has been used for the estimation of Mn, Na, and K in different varieties of oil seeds of mustard and sunflower in India. The samples were irradiated in a²⁵²Cf source with neutron flux of 10⁹ n s^–1 and the analysis was done using a multichannel analyzer (MCA) coupled to high purity germanium (HPGe) detector. Different varieties of seeds are found to have different concentrations of tracer elements when compared among themselves.     

An241Am−Be source based thermal neutron activation analysis facility at KFUPM

An instrumental thermal neutron activation analysis facility based, on a 16 Ci²⁴¹ Am–Be source, a high resolution -ray spectrometry setup and a PC-based data acquisition system at KFUPM is described. The thermal neutron flux distribution was determined from the induced activities of high purity indium foils. The absolute thermal neutron flux was calculated from the activities of bare and cadmium-covered gold foils at a position of 3 cm from the soource at which the flux reaches a maximum. The facility tests were carried out with the determination of manganese concentrations in six types of industrially important steel samples. The result of 1.33% manganese in SS-304 steel sample was in excellent agreement with the literature value. The method is nondestructive, economical and ideal for bulk analysis.     

Thermal neutron activation analysis of Cu in its ores by using an241Am−Be neutron source

A thermal neutron activation method has been developed for the determination of Cu in Cu–Pb–Zn ores and chalcopyrite ore concentrates using the reaction⁶³Cu(N, )⁶⁴Cu. The samples were irradiated with thermal neutrons from an²⁴¹Am–Be neutron source and the annihilation -radiations of 0.511 MeV were counted on 3×3 NaI(T1) detector coupled with single channel pulse height analyzer. The method is nondestructive, economical and ideal for bulk analysis of ores with 1–16% Cu.     

Uranium and thorium determination in Brazilian coals by epithermal neutron activation analysis

An experimental technique has been developed to determine impurities in coal. Uranium was determined by counting the²³⁹Np 106.1 keV -ray with a LEPS detector and thorium by counting the²³³Pa 311.8 keV -ray with a Ge(Li) detector. Seventeen coal samples were analyzed with an average precision of 3% and a quantitative determination limit of 0.153 g/g for uranium and 0.078 g/g for thorium. The technique allows determinations of up to twenty elements besides U and Th and can be applied in routine analysis.     

Determination of trace elements in Brazilian cigarette tobacco by neutron activation analysis

The determination of 14 trace elements /Ba, Ce, Co, Eu, Fe, Hf, La, Nd, Rb, Sb, Sc, Sm, Tb and Th/ has been carried out in three different brands of Brazilian cigarettes. The samples and standards were irradiated for 8 h at a thermal neutron flux of approx. 5×10¹² n cm^–2s^–1. After the irradiation, the -rays activity was measured on a Ge/Li/ detector coupled with a 4096-channel pulse height analyzer. The results were compared with those obtained for the tobacco from American, Iranian, Turkish, Pakistan and Yugoslavian cigarettes. The amount of each element transferred to the ashes was determined.     

Amperometric detection of heavy metal ions in ion pair chromatography at an array of water/nitrobenzene micro interfaces

A novel amperometric detector for heavy metal ions has been developed and successfully applied for ion pair chromatography. The detector is based on the electrochemical transfer of the metal ions across an array of water/nitrobenzene micro interfaces. The ion transfer is facilitated by the neutral ionophores methylenebis(diphenylphosphineoxide) and methylenebis(di- phenylphosphinesulfide). More than eight metals are separated in less than 15 min on an RP18 column using octyl sulfonate as ion pair reagent. For the heavy metals, the limits of decision are 19(Pb²⁺), 9(Zn²⁺), 9l (Co²⁺), 8(Cd²⁺) and 1.6(Mn²⁺) g/L. The applicability of the new method for water samples is demonstrated.     

Measurements of thermal neutron cross section and resonance integrals of74Se,75As,94Zr,134Cs,238U

The thermal neutron cross sections and resonance integrals of⁷⁴Se,⁷⁵As,⁹⁴Zr,¹³⁴Cs,²³⁸U have been measured. Neutron activation was performed by using the ICIS-flux position of the CONSORT-II Reactor. A high resolution -ray detector system was used to measure the reaction rates of the irradiated samples. Results of analysis are presented and compared with literature values.     

Fluorometric Determination of Nitrogen Dioxide in Atmosphere Sampled by the Liquid Droplet Technique

A new, simple, sensitive and selective fluorometric method for the determination of nitrite has been developed. The reaction of nitrite with hydralazine in acidic medium, heated on a boiling water-bath for 15 min, produced a tetrazolo (5,1-a) phthalazine (Tetra-P). The product formed was measured at _ex = 274 nm and _em = 345 nm. The fluorescence intensity was valid over a nitrite concentration range 0.067–60.3 ng mL^–1, with a detection limit of 0.0091 ng mL^–1. The reproducibility of the proposed method was determined by running a different concentration of nitrite, 13.4, 33.5, and 46.9 ng mL^–1. The % recoveries and the relative standard deviations were found to be 100.6 ± 0.9, 99.9 ± 0.5, and 99.4 ± 1.1%, respectively. The proposed method was applied successfully to the determination of nitrogen dioxide sampled from the atmosphere using the liquid droplet method. The nitrogen dioxide our wind tunnel was controlled by an NO _x analyzer based on a chemiluminescence analyzer detector (CLAD 1000). A linear graph was obtained for the nitrogen dioxide in the wind tunnel vs. NO₂ sampled by the liquid droplet method. The effect of interference substances in the determination showed that cations and anions did not disturb the process. The results obtained were satisfactory when compared with the reference method.     

Rapid radiochemical separation and determination of chlorine,bromine and iodine in water samples using ion exchange

On the basis of tracer experiments, a simple and rapid radiochemical separation method for simultaneous determination of I^–, Br^– and Cl^– in one aliquot of a water sample (only 2–4 ml) has been developed. The method is based on short irradiation of the water sample and separation of the halogens using sequential ion exchange columns filled with Dowex 1×8, 100–200 mesh anionic resin prepared in I^–/I₂, Br^–/Br₂ and Cl^– form. After washing the columns with an appropriate volume of 2% NaCl solution, the resins were transferred to vials and activities of the isolated radionuclides¹²⁸I,⁸²Br and³⁸Cl measured together with standards in a well type or on a coaxial Ge detector connected to a Canberra 90 multichannel analyzer. Besides high chemical yields, from the -spectra of the isolated radionuclides, it is evident that high decontamination fac-The paper was presented at the MTAA-8, Vienna, September 1991.     

Non-destructive determination of low-level210Pb and226Ra with an ordinary high-purity Ge-detector

A convenient non-destructive method for the determination of low level²¹⁰Pb and²²⁶Ra with an ordinary high-purity Ge-detector is presented. The ordinary Ge-detectors used in this work were available to measure 46.5 keV -rays of²¹⁰Pb. These detectors were also useful for the non-destructive analysis of low-level²²⁶Ra in lime-stone and calcium chemicals when a stream of nitrogen gas was maintained around the detectors. By this method, measurements could be carried out not only for²¹⁰Pb and²²⁶Ra but also for other -emitting radionuclides simultaneously, using the same detector. The detection limits of about 1 Bq per sample for²¹⁰Pb and about 0.05 Bq per sample for²²⁶Ra, respectively, were estimated, when the samples were counted for 1–2 days.     

Voltammetric Detector for Liquid Chromatography: Determination of Triclosan in Rabbit Urine and Serum

A flow-electrolytic cell containing a strand of carbon fibers has been designed and characterized for use in a voltammetric detector for high-performance liquid chromatography. The detector was used for determination of triclosan (2,4,4-trichloro-2-hydroxydiphenyl ether) in rabbit serum and urine. Analysis of rabbit serum and urine 1 day and 1 to 5 days, respectively, after ingestion of oral triclosan revealed that the concentration of triclosan was higher than for control serum and urine. The concentration reached maximum levels after 6 h and 34 h or 44 h in serum and urine, respectively. When triclosan was determined in rabbit samples with the method proposed the results obtained were comparable with those obtained by high-performance liquid chromatography with ultraviolet detection.     

Gamma-spectrometric determination of uranium isotopes in biofuel ash

Gamma-ray measurements have been performed on biofuel samples using a planar intrinsic Ge detector. The samples were first homogenized and then packed into 90 ml plastic tubs. The radiation from each sample was usually measured for 1 to 2 days. The intensity of the 63.3 keV -ray in²³⁴Th was used to determine the amount of²³⁸U present. The amount of²³⁵U can be determined from the intensity of the 143.8 keV -ray.     

Uses of PGAA at the Dalat reactor

A facility for neutron capture prompt -ray spectroscopy for activation analysis has been intstalled at the tangential beam tube of the 500 kW Dalat reactor. Using a single crystal of silicon for filtering the thermal neutron beam and the 73 cm³ HP-G detector shielded by common materials with flexible configurations suitable to various samples, LOD of nearly 30 elements were estimated. Applications of PGAA in the determination of elemental concentrations in biological, environmental, geological and industrial product samples are presented.