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%.     

Neutron activation analysis of manganese and nickel in commercial steel samples

The non-destructive thermal neutron activation analysis of some commercially available steel samples viz. SS-316, SS-310, SS-304, Tiscral, CA55 and EN 8 is carried out using a²⁵²Cf source. The manganese content of these steel samples is estimated by measuring the -activity of⁵⁶Mn using a single channel analyzer on integration mode and a NaI/Tl/ detector as well as using a high purity germanium detector coupled to a 4K multichannel analyzer. The results obtained by both procedures show reasonable agreement with each other. The nickel content of the various steel samples is also estimated.     

Instrumental neutron activation analysis of air filter samples

Résumé La mesure de traces d'éléments dans l'air ambiant a fait l'objet d'une attention accrue ces derniers mois, en raison d'un intérêt grandissant pour les dangers en puissance pour la santé, qui résultent de l'exposition prolongée à certaines substances toxiques. L'analyse par activation neutronique a été employée avec succès dans la recherche de traces d'éléments, et ce, pour un grand nombre d'études de l'environnement; elle semble convenir de fa?on idéale pour la détermination non-destructive multi-élémentaire de la composition de milieux de particules portées par l'air. Dans cet article, on rend compte des performances de l'analyse instrumentale par activation neutronique comme on le montre dans le cas de 40 échantillons d'air filtrées provenant d'une zone métropolitaine.      

Radio-isotope neutron activation analysis for vanadium,manganese and tungsten in alloy steels

An instrumental neutron activation method for V, Mn and W in alloy steels with a ²⁴¹ Am/Be isotopic neutron source is described. The samples were irradiated to induce the nuclear reactions ⁵¹V(n, γ) ⁵²V, ⁵⁵Mn(n, γ)⁵⁶Mn, and ¹⁸⁶W(n, γ)¹⁸⁷W. The activities were measured with a NaI(TI) detector. Interferences on the measured photopeaks were shown to be negligible by measuring the half-lives of ⁶²V, ⁵⁶Mn and ¹⁸⁷W.These thre elementes were determined in the range 1.5–12.9% in special steels; manganese in the range 0.5–1.6% was measured in cast irons. Calibration was done by comparison with results from wet chemistry and x-ray fluorescence spectrometry. The processing times for the vanadium, manganese and tungsten determinations were 11 min, 3 h and 26.3 h, respectively, but these were reduced greatly by intoruding a scheme wherein six samples were simultaneously irradiated and the ⁵⁶Mn and ¹⁸⁷W nuclides were measured sequentially for a series of 66 samples. The average processing time was reduced to 45 min for tungsten with a precision of 4.0% and accuracy of 3.4% and 22.8 min for manganese with a precision of 3.8% and accuracy of 3.1%.     

Instrumental neutron activation analysis of some rock samples from Akwana and Arufu areas,Middle Benue Trough,Nigeria

Twenty nine (29) major, minor and trace elements including rare earth elements (REEs) were determined by INAA in rock samples from Akwana and Arufu areas, Middle Benue Trough, Nigeria. The rock units are located within the lead-fluorite and baryte mineralisation there. The concentrations of the major elements in the tertiary basalt (TB) and dolerite are similar while the elemental abundance in the granite gnesses is completely different. The elemental concentrations in the rock samples do not show any known relationship with fluorite abundance. The concentrations of some elements in both tertiary basalt and dolerite show them to be derived from alkali basaltic liquid. The chondritic normalised REE distribution patterns for the TB are similar to those of BCR-1 but the chondritic relative REE abundance is more enriched in TB than in the BCR-1. The chondritic normalised REE distribution patterns for the granite gneisses are also compared to those of the standard granite samples.     

Instrumental neutron activation analysis for multi-elemental determination in Indian tea samples

Instrumental neutron activation analysis (INAA) was employed to determine concentrations of 19 elements (As, Ba, Br, Ce, Co, Cr, Cs, Fe, K, La, Mn, Na, Nd, Rb, Sc, Sm, Th, Yb and Zn) in a large number (55) of tea samples (from market as well as virgin tea leaves) from different locations in India (Assam, Darjeeling, Munnar and Kangra). The results obtained in the present work are compared with those reported in literature. The concentration levels, their variations with collection locations and the correlations among different elements in these samples are discussed.     

Instrumental neutron activation analysis of large samples: A pilot experiment

A large sample INAA (LS-INAA) was conducted based on available experimental conditions. Four different materials, e.g., a quartz-sand and three wastes from an incineration plant were analyzed on sample size of 1 kg. The neutron flux spatial distribution was determined by irradiation of flux monitors in the sample. The gamma-ray apparent counting efficiency was evaluated based on the effective-solid angle concept, using linear attenuation coefficients calculated from an iteration process. The k ₀- and the modified monostandard methods were modified for the LS-INAA. To check the LS-INAA performance, a conventional small sample INAA was carried out for the quartz sand and a waste. All detected elements in the LS-INAA are presented and the discussion is conducted to explore the sources of errors in the LS-INAA. As a pilot experiment, the information from this work will be used in constructing irradiation and counting devices for the new FRM-II neutron source in Garching, Germany.     

Instrumental neutron activation analysis of native copper: Some methodological considerations

A scheme for INAA of native copper, which permits the determination of 22–24 elements is proposed. The possible error source in INAA of native copper and other types of more or less pure copper are evaluated quantitatively. The accuracy and precision of the analyses are tested by comparison with NIST-SRM's. The applicability of the proposed method for archaeometric investigations is demonstrated by the analysis of two samples of native copper and two eneolithic archaeological artifacts from Bulgaria.     

Instrumental neutron activation analysis of some ancient punchmark coins from India

A nondestructive instrumental neutron activation analysis technique is applied for the analysis of precious ancient punchmark coins. Coins ranging between 8th century B.C. to 2nd century B.C. were irradiated with thermal neutrons in a²⁵²Cf neutron source facility and analyzed by comparator method of instrumental neutron activation analysis, using high purity germanium detector coupled to a multichannel analyzer, the activities being measured at photopeak energies of the corresponding radioisotopes. It is observed that punchmark coins are mainly of two types: copper or silver based. Other elements present in varying proportions are gold, arsenic and antimony.     

Instrumental neutron activation analysis of geological and pedological samples. Further investigation of epithermal neutron activation analysis using monostandard method

A comparative study is presented on neutron activation analysis of rock and soil samples using whole reactor neutron spectrum and epithermal neutrons with both relative and monostandard procedures. The latter procedure used with epithermal neutron activation analysis of soil samples necessitated the use of the “effective resonance integrals” which were determined experimentally. The incorporation of the β factor, representing deviation of reactor epithermal neutron flux from 1/E law, is developed in the present work. The main criteria for the choice of one or more of the procedures studied for a given purpose are also indicated. Analysis of 15 trace elements, Ca and Fe in the standard Japanese granite JC-1 using monostandard epithermal neutron activation gave results in good agreement with the average literature values. This paper is dedicated to the 80th birthday of Professor Dr. Robert Klement, University of Munich.     

Instrumental neutron activation analysis of samples with masses from micrograms to hectograms

The rotating rig at the Danish DR-3 reactor was used for irradiation of samples with masses from a hundred micrograms to several hundred grams. The pneumatic post for uranium delayed neutron counting was used for automatic sequential irradiation of samples subdivided into up to 24 aliquots, each with a volume of 7 cm³. The cumulative samples were measured in polyethylene irradiation containers in a specially designed radial holder.     

Instrumental neutron activation analysis of environmental samples using thek 0-standardization method

The use of thek ₀-standardization method in instrumental neutron activation analysis gives good accuracy and precision. The analysis time can be reduced drastically by employing software for thek ₀-standardization calculations. In this work samples were irradiated in a TRIGA reactor and the gamma spectrum was analysed by Sampo 90 and thek ₀-standardization by the KAYZERO/SOLCOI code (DSM Research). The efficiency measurement and the peak to total ratio at the reference and other geometries were measured and tested for their accuracy by analysing some reference materials. Reference materials such as SRM 1572 (Citrus leaves), SRM 1573 (Tomato leaves), SRM 1575 (Pine needles), IAEA Soil-7 (Soil) and SRM 1646 (Estuarine sediment) were analysed for the major, minor and trace element contents. The results were in good agreement with the certified or literature values. The recently released IAEA 140 (Sea plant homogenates) was also analysed for 28 elements.     

Determination of copper in biological samples by substoichiometric neutron activation analysis

A method has been described for the determination of trace amounts of copper in biological samples by thermal neutron activation analysis, involving radiochemical separation of copper from irradiated matrix employing substoichiometric extraction of Cu/II/ with 2-mercaptobenzothiazole /2-HMBT/ into chloroform. 4.01 g of Cu/II/ can be determined with an accuracy of 3.13% and precision of 1.08%.     

Instrumental neutron activation analysis of a sulfide ore and some ore benefication products

Samples of a pyritic lead-zinc ore and some benefication products were examined by instrumental activation analysis using Ge(Li) gamma-spectrometry. The following elements were determined using thermal neutron activation: Sc, Cr, Co, Zn, As, Se, Ag, Sb, Ir, Au and Th. The technique is especially favourable for the determination of cobalt, arsenic, antimony and gold, but selenium, silver and thorium can also be determined in most fractions. Activation with epithermal neutrons will improve conditions for the determination of As, Sb, Se, Ag, Au and Th.     

Instrumental neutron activation analysis of samples with volumes from 2 to 350 ml

Usually neutron activation analyses are performed in point-source geometry. However, specially designed irradiation positions and carefully planned measuring conditions enabled the activation and analysis of samples with weights up to several tens of kilograms. A dedicated character of irradiation and of measuring conditions was the main reason for a very limited application of such activation analysis. The use of routine irradiation facilities and standard conditions for analytical gamma-spectrometric measurements is described. Starting with samples of some hundred milligrams usually used in activation, through multi-gram samples to several hundred gram samples, irradiation and measuring conditions were studied and tested for development of the method. This work began in 1991 in Denmark, using the Danish DR-3 reactor. Since then different aspects of the method have been investigated on 6 reactors; in Denmark on DR-3, in Austria on Triga-MkII (in Vienna), and Astra (in Seibersdorf), in the German Federal Republic on FRG-1 in Geesthacht, in Norway on Jeep II (in Kjeller), and in Kazakhstan on VVR-K (in Alatau). Altogether more than 1000 samples have been irradiated and measured. In total, the roughly 30 kg of irradiated materials included almost 300 large samples of more than 30 gram weight. The following theoretical and practical aspects were investigated during the work: theoretical problems concerning neutron self-absorption in common organic and inorganic materials, as well as gamma-attenuation during the measurement. From a more practical point of view: health physics and radiation hazards during irradiation, measurement, transportation and storage of samples with several hundred grams weight. Special requirements to irradiation containers were formulated and various containers were tested. Main advantages and drawbacks of the method are discussed.     

Instrumental neutron activation analysis of urinary calculi

Five kinds of urinary stones from 42 patients have been determined for a total of 19 elements by instrumental neutron activation analysis. Of these elements, Ca, Mg, Sr, Na, and Cl are found to be present in the core of all kinds of stones. The differences in elemental composition among the different kinds of stones as well as across the layers of stone are statistically evaluated.     

Instrumental neutron activation analysis of brewer's yeast

Instrumental neutron activation was used for the determination of 23 trace and minor elements in 4 different samples of brewer's yeast. Detection limits for these elements vary from 2 ppb to 100 ppm. The following average concentrations were found (ppm, dry weight): Al 597, Br 0.36, Cl 1473, Co 0.21, Cu 19, Fe 285, K 16 400, Mg 1355, Mn 8.4, Na 2330, Rb 19, Sb 0.053, Se 1.2, V 2.2 and Zn 80. NBS standard 1569 was also analyzed and the following concentrations (in ppm) were measured: Al 2300, Br 0.65, Ce 0.23, Cl 460, Co 0.26, Cr 2.12, Cu 11, Fe 707, Gd 7.1, Hf 0.13, K 15 500, Mg 1780, Mn 7, Na 510, Rb 16, Sb 0.075, Sc 0.18, Se 0.92, Th 3.7, Ti 38, U 0.49, V 4.1 and Zn 70.     

Instrumental neutron activation analysis of gunpowder residues

A procedure has been developed for the detection of gunpowder residues deposited on the hand of a person firing a gun. The method is based on neutron activation analysis of the antimony level on the surface of the hand. The surface materials are removed by a film made by spraying a 4% solution of cellulose acetate in acetone, which sets to form a thin film that can readily be stripped off. This technique was found to be preferable to the paraffin-lift technique which is in common use. Following neutron activation of the film in a nuclear reactor, antimony is assayed by high-resolution Ge(Li) spectrometry without prior chemical processing. The sensitivity of the method is about 5·10⁻⁹ g Sb, with a precision of about ±10% at a neutron flux of 5·10¹³ n·cm⁻²·sec⁻¹. Analysis of twenty samples taken from the hands of persons who had fired a pistol gave Sb levels of 0.4±0.2 μg, compared with 0.024±0.013 μg found on the hands of persons who had not fired a revolver. The possible extension of the present technique to include the determination of additional elements is discussed. Project carried out with the support of the Office of the Chief Scientist to the Ministry of Defense and with the collaboration of the Israel Police.