Fast neutron activation: Sample preparation utilizing graphite as a diluent

A method has been developed for the preparation of irradiation samples which ensures that both standard and unknown samples are of the same size, shape, density and composition. Powdered standard and unknown samples were diluted with graphite to give homogeneous mixtures containing ≥80% graphite; these mixtures were pressed into cylindrical pellets. This method of sample preparation has been applied to the determination of nitrogen in organic and polymeric compounds. The results generally agree with Kjeldahl analyses within 5%. This work was supported by the United States Atomic Energy Commission.     

Determination of lithium in graphite by neutron activation analysis

Trace impurities of lithium in graphite is one of the sources of tritium in high-temperature reactors. To determine contents of less then 1ng/g a procedure based on the (n,)-reaction of⁶Li was developed. The samples are irradiated in a reactor and then ignited in a Wickbold apparatus. Thereby the tritium produced by the (n,)-reaction is completely converted in HTO, which can be easily purified by distillation and, if necessary, by a scavenger precipitation step. Several types of graphite have been investigated and the lowest content measured was 0.2 ng/g.     

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.     

Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry

A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH₄OH+0.05% w/v Triton X-100^®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO₃)₂ as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1⁻¹ Se, corresponding to 30 μg l⁻¹ Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l⁻¹, with a mean value of 114±22 μg l⁻¹.     

Polyaniline as a base material for preparation of a mercury standard for use in neutron activation analysis

Polyaniline sorbed with microgram quantity of mercury was prepared and its homogeneity and stability with respect to mercury was evaluated over a period of time. The volatilisation loss of mercury during and after neutron irradiation was studied. It was found that polyaniline was homogeneous and stable with respect to mercury. No loss of mercury from polyaniline was observed during and after neutron irradiation. Thus polyaniline sorbed with mercury can serve as a good standard for neutron activation analysis of mercury.     

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.     

Instrumental neutron activation analysis of graphite electrode of dry battery

Neutron activation analysis has been applied for determination of trace elements in graphite electrode of dry batteries as a forensic-bomb debris. Eleven samples collected in Japan were analyzed nondestructively. Fourteen elements (As, Ce, Co, Cr, Cs, Fe, K, La, Na, Sc, Sm, Th, W, and Zn) were determined and their elemental compositions were compared for their differentiation.     

Accuracy in standards preparation for neutron activation analysis

Errors in preparing standards, especially multielemental standards, are extremely important if accurate results are desired from neutron activation analysis (NAA). It is often convenient to prepare standards for NAA from single or multi-element solutions which are then deposited onto (or into) a suitable matrix, such as filter paper or quartz vials. There are many potential sources of error in preparing single-element standards including: impurities and non-stoichiometric composition of the element or compound used to prepare the standard solutions; evaporative losses of solvent; inaccuracy of calibration, and imprecision of the pipettes used; moisture content of elements or compounds used; contamination from reagents, equipment, laboratory environment, or final matrix of the standard; instability of standard solutions (i.e., to losses via precipitation or adsorption), and losses of volatile elements during dissolution and/or irradiation. Additional sources of error in preparing multielement standards includes: instability of mixed, multielement solutions, and cross-contamination of one element by the addition of a second element. Procedures previously used by the author at NIST to prepare multielement standards with concentrations accurate to about one percent are described. Additional techniques needed to prepare multielement standards with accuracies better than 1 percent will be discussed.     

Thermal and epithermal neutron activation analysis using the monostandard method

A new approach is presented for neutron activation analysis using the monostandard (single comparator) method. Elements to be determined are classified into two groups; those with σ_o>I_o are activated with whole neutron spectrum (without Cd-cover), using a standard of the same group (e.g. Sc), while elements with I_o>σ_o are activated with epithermal neutrons (under Cd-cover) using a standard of the same group (e.g. Au or Co). Epithermal activation increases the number of determinable elements and its coupling with the monostandard method has the advantage of using a small Cd-cover. The σ_o and I₀ values of some elements were determined to test this approach.     

Thermal neutron activation analysis of hafnium in zircaloy with a Van de Graaff accelerator

Thermal neutron activation analysis of hafnium in zircaloy was investigated with a Van de Graaff accelerator. Thermal neutrons were obtained by moderating Be−D fast neutrons with paraffin blocks.^179mHf isotope with a half-life of 18.6 s, produced by¹⁷⁸Hf(n, γ)^179mHf reaction, was utilized in the present analysis. This method made it possible to analyze hafnium rapidly and non-destructively by using scandium as an internal standard material. Several tens to hundreds of ppm of hafnium in zircaloy samples were determined within 2 minutes with a precision of about ±1%.     

Modified soybean oil as a reactive diluent: Synthesis and characterization

Soybean oil was modified in two steps: (1) conjugation of soybean oil and (2) Diels‐Alder addition with 3‐(trimethoxysilyl)propyl methacrylate, 2,2,2‐trifluoroethyl methacrylate and triallyl ether acrylate. The structures were characterized using ¹H NMR, ¹³C NMR, ¹³C‐¹H gradient heteronuclear single quantum coherence (gHSQC) NMR spectroscopy, and MALDI‐TOF mass spectrometry. The ¹³C‐¹H gHSQC NMR spectra helped confirm the formation of a cyclohexene ring in all reactions, indicating a Diels‐Alder addition. The diluent efficiency of modified soybean oil was evaluated in long oil alkyd formulation. Triallyl ether functionalized soybean oil resulted in the highest reduction in the viscosity of the alkyd formulations. © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 3045–3059     

Instrumental neutron activation analysis of lanthanides and other elements employing CIRUS reactor as a thermal neutron source

The high thermal neutron flux provided by the CIRUS reactor (1×10¹³ n cm^–2s^–1) has been used to determine elements having long half-lives or poor thermal neutron crosssections. Selective cooling time and the use of a high resolution HPGe detector in conjunction with a PC based MCA unit have made it possible to analyze many elements in a single irradiation run. The method developed has been used for the analysis of ores such as Ilmenite, Rutile, Sillimanite, Garnet, Zircon and Monazite.     

Beta-exposure in a neutron activation laboratory

Summary In virtually all neutron activation analysis laboratories, researchers are given film badges known as thermoluminescence dosimeters (TLD's) that are monitored on a monthly basis. Sometimes additional pocket dosimeters are worn to get a daily reading of exposure, while in other instances ring badges are worn to assess beta doses. However, more than often little consideration is given to beta-exposure rates that arise from the plethora of radionuclides produced in the many types of samples irradiated. A common mistake is to assess gamma-exposures of activated samples that rely on the use of a beta-shield on the survey meter. Our experimental results have shown that there are many high energy beta-particles from neutron activated samples that can easily penetrate the beta-shield and thus give an underestimation of the total beta-exposure.     

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.     

Instrumental neutron activation analysis of Al,V and Ti employing252Cf as a thermal neutron source

A rapid method for the determination of Al, V and Ti has been developed and is used for the analysis of these elements in different ores and alloys. An isotopic neutron source²⁵²Cf having a thermal neutron flux of the order of 8.5×10⁷ n·cm^–2 sec^–1 has been used for thermal neutron bombardment. Activity measurements were performed on a HPGe detector coupled to a PC based MCA unit. Depending on the half-life of the (n, ) product, different irradiation and cooling times were employed and thus the elements of interest were analyzed sequentially.     

Thermal reduction of graphite oxide derivatives for preparation of supports for platinum hydrogenation catalysts

Thermal reduction of graphite oxide and its derivatives under argon atmosphere has been studied by means of thermogravimetric analysis. Carbon materials prepared via thermal reduction of graphite oxide derivatives in argon at 900°С during 3 h have been used for deposition of platinum from H₂PtCl₆ solutions. Pt particles supported on the support catalyze liquid-phase hydrogenation of nitrobenzene and dec-1-ene under atmospheric pressure of H₂. Thermal reduction of the supports based on graphite oxide results in the formation of the structural defects significantly enhancing the catalytic activity.     

Instrumental neutron activation analysis as a means of evaluation of reference sample homogeneity

Homogeneity is the first and most essential prerequisite of a reference material which merits this marking. A possible way to do homogeneity tests on many elements is offered by instrumental neutron activation analysis. It is shown that this method allows the quick evaluation of sample homogeneity on very small samples and for many elements simultaneosly, regarding macro as well as ultra trace elements.