Evaluation of 40K in food by determining total potassium using neutron activation analysis

Summary Potassium is an extremely important major element to the human body. Potassium is made up of three isotopes with abundances of ³⁹K at 93.1%, ⁴⁰K at 0.0118% and ⁴¹K at 6.88%. It is also very well known that ⁴⁰K with its 1.3 ^. 10⁹ years half-life is a major naturally occurring isotope in the body and food. The usual way to determine total ⁴⁰K is to measure the single 1460.8 keV photon from beta-decay. However, this procedure requires a significant amount of sample and typical counting periods of at least a day in well-shielded germanium counting system. Another approach is to determine total potassium via neutron activation analysis using the well known ⁴¹K(n,g)⁴²K (T_1/2 = 12.8 h) reaction and then evaluate ⁴⁰K using the usual activity equation A = lN. In our laboratory we have effectively used epithermal neutron activation analysis and Compton suppression to determine potassium in air filters and other geological material. Upwards to 10-15 samples can be analyzed in one day using only gram quantities of material. In such way one can increase the output of determining ⁴⁰K by at least one order of magnitude. Results of a detailed investigation optimization of the methodology, quality control and detection limits will be presented for reference material and various food samples.     

U determination in environmental samples by delayed neutron activation analysis in Korea

A delayed neutron counting system has been implemented at the HANARO research reactor in 2007. Thermal neutron flux measured at the NAA #2 irradiation hole coupled to the delayed counting system, was higher than 3 × 10¹³ n cm⁻² s⁻¹. The delayed neutron counting system is composed of 18 ³He detectors which are divided into three groups with six detectors and the collected signals of each group are processed to a digital signal. The count numbers were measured with the uranium mass by using NIST SRMs under fixed analytical condition and their correlation could be determined. Finally, delayed neutron activation analysis has been carried out for the determination of uranium mass fraction in the collected environmental samples.     

Measurements of the thermal neutron cross-sections and resonance integrals for 186W (n,γ) 187W and 98Mo (n,γ) 99Mo reactions

The thermal neutron cross-sections and resonance integrals of the ¹⁸⁶W (n,γ) ¹⁸⁷W and ⁹⁸Mo (n,γ) ⁹⁹Mo reactions in the thermal and 1/E regions, respectively, of a thermal reactor neutron spectrum have been experimentally determined by the activation method using ¹⁹⁷Au (n,γ) ¹⁹⁸Au reaction as a single comparator. The high purity natural W, Mo, and Zr foils; and Au wire diluted in aluminum, were irradiated without Cd shield in two neutron irradiation sites, characterized with different values for the thermal-to-epithermal flux ratios, f at the Second Egyptian Research Reactor (ETRR-2). The induced activities in the samples were measured by high-resolution γ-ray spectrometry with a calibrated germanium detector. Thermal neutron cross-sections for 2200 m/s neutrons and resonance integrals for the ¹⁸⁶W (n,γ) ¹⁸⁷W and ⁹⁸Mo (n,γ) ⁹⁹Mo reactions have been obtained relative to the reference values, σ₀ = 98.65 ± 0.09 b and I ₀ = 1500 ± 28 b for the ¹⁹⁷Au (n,γ) ¹⁹⁸Au reaction. The necessary correction factors for thermal neutron and resonance neutron self-shielding effects, and the epithermal flux index (α) were taken into account in the determinations. The results obtained were: σ₀ = 38.43 ± 0.4 b and I ₀ = 502 ± 65 b for ¹⁸⁶W (n,γ) ¹⁸⁷W, and σ₀ = 0.137 ± 0.014 band I ₀ = 6.47 ± 0.8 for ⁹⁸Mo (n,γ) ⁹⁹Mo. These results are discussed and compared with previous measurements and evaluated data in literature. The traditional method of determining thermal cross-sections and resonance integrals via neutron irradiation with and without Cd shield in one irradiation position was avoided in this work by neutron irradiation without Cd shield in at least two different neutron irradiation positions. This method provides alternative way for determining thermal cross-sections and resonance integrals simultaneously.     

A brief introduction to NAA facilities of China Advance Research Reactor at CIAE

China Advance Research Reactor (CARR) at China Institute of Atomic Energy (CIAE), with a non-perturbed maximum thermal neutron flux of 1 × 10¹⁵ cm⁻² s⁻¹ at the center of active area, is one of the most powerful research reactors in the world. Three neutron channels have been allocated for conventional neutron activation analysis (NAA), thermal neutron prompt gamma activation analysis (PGAA) and cold neutron PGAA, respectively. Two irradiation tube systems are installed in the conventional NAA channel. One of them is for short irradiation with the rabbit size of diameter (Φ)19 × 40 mm, the other one is for long irradiation with the rabbit size of Φ39 × 70 mm. The medium temperature is about 45 °C and the thermal neutron flux is about 3 × 10¹⁴ cm⁻² s⁻¹ at sample positions. The flux gradient is expected to be very small according to the designed neutron flux distribution. Pneumatic systems are used for samples transfer. The speed of rabbits is designed to be about 20 m/s, and it takes 3 s to travel from irradiation position to detector. Three sets of gamma counting systems and one delayed neutron counting system are being equipped for routine analysis. They are designed for running continuously and automatically. And all the functions can be operated at laboratory or office through remote controlled computer. Software has been made domestically for spectrum peak search, concentration calculation with relative method and k₀ method with interference corrections and some other functions for the convenience of users.     

Investigation of fast neutron shielding characteristics depending on boron percentages of MgB<Subscript>2</Subscript>, NaBH<Subscript>4</Subscript> and KBH<Subscript>4</Subscript>

The macroscopic cross-section Σ and average neutron fluence in matter Φ are usable factors to comment neutron shielding property of samples. In this paper, we have used MgB₂, NaBH₄ and KBH₄ samples including different percentages of boron. Neutron macroscopic cross-section measurements of them have been done by using a source of mono-energetic neutrons (E _eff = 4.5 MeV ²⁴¹Am–Be). Average neutron fluence values and double differential fast neutron flux distributions of each samples calculated by using FLUKA Monte Carlo code. Also half value layers (HVLs) of samples are compared to paraffin which is one of the most neutron moderators. As a result, growing boron concentration can raise neutron shielding property of materials.     

The pressure effect study on the burning rate of ammonium nitrate-HTPB-based propellant with the influence catalysts

The burning rate of AN–HTPB-based propellant catalysed with chromium salt has been studied using conventional strand burner under the various pressure range, i.e. from atmospheric pressure to 6.897 MPa and verified with Piobert law, i.e. r = aP ⁿ . At atmospheric pressure, the burning rate AN–HTPB propellant was being accelerated with the chromium-based catalysts used. In case of lead chromate-catalysed system, burning rate was observed 2.655 times higher than burning rate (r = 0.200 mm s⁻¹) of virgin AN–HTPB propellant sample. However, the Copper chromate-catalysed propellant burned with slower rate (r = 0.160 mm s⁻¹) than the virgin AN–HTPB propellant sample. The burning rate of all catalysed propellant samples are found to be the pressure sensitive and accelerated higher with rise of pressure. The highest burning rate (r = 2.422 mm s⁻¹) was recorded with ammonium dichromate and lowest (r = 1.40 mm s⁻¹) with lead chromate-catalysed propellant sample with the rise of pressure up to 6.897 MPa at different pressures. A linear relationship was observed between the burning rate and pressure rise which followed the Piobert law, i.e. r = aP ⁿ . The pressure index (n) values of AN–HTPB-based samples were calculated higher when catalysed with ammonium dichromate, Copper Chromate, Cr₂O₃, Potassium dichromate (n = 0.525, 0.555, 0.429, and 0.408 respectively) and lower (n = 0.226) with lead chromate compared to virgin sample (n = 0.405). Higher value indicates the positive effect on accelerating the burning rate with catalyst at higher pressure ranges.     

Liquid scintillation measurement of40K for the education on radioactivity

Liquid scintillation counting of⁴⁰K in ordinary potassium propionate is a highly suitable experimental task in the general education on radioactivity. The counting efficiency is about 90%, depending little on the measurement conditions. Potassium propionate is of suitable properties and can be easily obtained commercially or by conversion from other compounds. The result of counting, about 1,700 cpm/g, is highly impressive to many students, indicating the existence of⁴⁰K radioactivity unexpectedly high in the normal nature, and can be used for the exercise of calculating our internal radiation exposure.     

<Superscript>40</Superscript>K activities and potassium concentrations in tobacco samples of Mexican cigarettes

Nine brands of tobacco cigarettes manufactured and distributed in the Mexican market were analyzed by γ-spectrometry to certify their non-artificial radioactive contamination. Since natural occurring radioactive materials (NORM) ⁴⁰K, ²³²Th, ²³⁵U, and ²³⁹U (and decay products from the latter three nuclides) are the main sources for human radiation exposure, the aim of this work was to determine the activity of ⁴⁰K and potassium concentration. Averages of ⁴⁰K and potassium concentration were of 1.29±0.18 Bq·g⁻¹, and 4.0±0.57%. The annual dose equivalents to the whole body from ingestion and inhalation of 26 Bq ⁴⁰K were 0.23 μSv and 15.8 μSv, respectively. The corresponding 50 years committed dose equivalents was 0.23 μSv. The total committed dose to the lungs due to inhalation of ⁴⁰K in tobacco was 16 μSv. Potassium concentrations obtained in this work were in the same range of those obtained by INAA, so showing that the used technique is acute, reproducible, and accessible to laboratories equipped with low background scintillation detectors.     

Cyclic neutron activation analysis for determination of selenium in food samples using <Superscript>77m</Superscript>Se

Cyclic neutron activation analysis method was conducted for determination of Se in food samples. High accuracy and good precision were proved by analyzing certified reference materials (CRMs) of chicken (GBW10018), rice (GBW10010) and cabbage (GBW10014). The detection limits for the three CRMs reached 0.16, 0.66 and 1.2 ng after 6 cycles at the 161.9 keV γ-peak from ^77mSe, under a neutron flux of 9.0 × 10¹¹ n cm⁻² s⁻¹ and the conditions of 30 s irradiation, 2 s decay, 30 s counting and 2 s waiting, significantly lower than those of conventional neutron activation analysis without any cycles, which were 0.94, 3.6 and 4.3 ng, respectively.     

Assessment of natural radioactivity in silt samples from Moticher lake near Kakrapar Atomic Power Station,India

The naturally occurring radioisotopes such as ²³⁸U, ²³²Th and ⁴⁰K in the silt samples collected from Moticher lake, Gujarat were evaluated. The activity of ²³⁸U, ²³²Th and ⁴⁰K was found to be 4.4-9.7 Bq kg⁻¹ with a mean 6.4 ± 1.3 Bq kg⁻¹, 10.5–21.2 Bq kg⁻¹ with a mean 15.6 ± 2.5 Bq kg⁻¹ and 102–231 Bq kg⁻¹ with a mean 160 ± 40 Bq kg⁻¹, respectively. The depth profile study could not reveal any significant vertical correlation on radioactivity levels of ²³⁸U, ²³²Th and ⁴⁰K. Radium equivalent activity (Ra_eq), external hazard index (H _ex) and internal hazard index (H _int) were calculated by using the activity of ²³⁸U or ²²⁶Ra, ²³²Th and ⁴⁰K in silt samples. Annual Effective Dose Equivalent (AEDE) level in Moticher silt was found to be 24.8 ± 5.0 μSv year⁻¹, which is much lower than the worldwide average value. The relative contribution to dose due to ²³⁸U and ²³²Th series were found to be 14% and 53%, followed by the contribution of 33% due to ⁴⁰K.     

A low-temperature heat capacity study of natural lithium micas

Low-temperature heat capacity of natural zinnwaldite was measured at temperatures from 6 to 303 K in a vacuum adiabatic calorimeter. An anomalous behavior of heat capacity function C _p(T) has been revealed at very low temperatures, where this function does not tend to zero. Thermodynamic functions of zinnwaldite have been calculated from the experimental data. At 298.15 K, heat capacity C _p(T) = 339.8 J K⁻¹mol⁻¹, calorimetric entropy S ^o(Т) – S ^o(6.08) = 329.1 J K⁻¹ mol⁻¹, and enthalpy Н ^o(Т) − Н ^o(6.08) = 54,000 J mol⁻¹. Heat capacity and thermodynamic functions at 298.15 K for zinnwaldite having theoretical composition were estimated using additive method of calculation.     

Selenium and mercury determination in biological samples using gamma–gamma coincidence and Compton suppression

Biological materials containing trace amounts of mercury and selenium were examined using neutron activation analysis. They were analyzed using Compton suppression and γ–γ coincidence counting. The 279 keV photopeak of activated mercury (²⁰³Hg) was analyzed in order to observe the mercury content in these samples. Selenium, an element found in many biological samples, interferes with the analysis of ²⁰³Hg when activated (⁷⁵Se). Because the selenium interference comes from a cascading emission, Compton suppression was utilized to reduce this interference. In order to fully characterize the selenium content in the samples, γ–γ coincidence was used which reduced the background and eliminated bremsstrahlung interference produced from neutron activated phosphorous through the ³¹P(n, γ)³²P reaction which is a pure beta emitter. As a result, we determined the mercury and selenium concentrations in three standard reference materials, which contain varying ratios of mercury to selenium concentrations. This study also showed that these types of concentrations can be determined from small (<500 mg) sample masses. Further work needs to be done on wet samples that require dehydration, as mercury can be lost through this process.     

Serum aluminum determination by instrumental neutron activation analysis in long-term haemodialysis patients

Serum aluminum levels were determined by instrumental neutron activation analysis in 31 patients undergoing long-term haemodialysis. Aluminum-28 1.778 MeV (T _1/2=2.24 min) γ-rays produced by the thermal neutron reaction²⁷Al(n,γ)²⁸Al were detected. Successive irradiation of the samples at epithermal neutron fluence was performed to correct for the interference from the fast neutron reaction³¹P(n,α)²⁸Al. Serum aluminum level in this group of subjects was adequately represented by a lognormal distribution with a mean and variance of 16.5 μg/l and 16.8 μg/l, respectively. The results obtained were found to be in agreement with serum aluminum determination performed by electrothermal atomic absorption spectrophotometry (r ²=0.97). Instrumental neutron activation can provide a rapid technique to routinely monitor long-term haemodialysis patients in order to identify individuals at greater risk to develop aluminum toxicity.     

Measurement of reaction cross-sections for 64Ni(n, γ) 65Ni at E n = 0.025 eV and 58Ni(n, p) 58Co at E n = 3.7 MeV

The reaction cross-sections for ⁶⁴Ni(n, γ) ⁶⁵Ni at E _n  = 0.025 eV and ⁵⁸Ni (n, p) ⁵⁸Co at E _n  = 3.7 MeV have been experimentally determined using activation and off-line γ-ray spectrometric technique. The thermal neutron flux used is from the thermal Column of the reactor APSARA at BARC, Mumbai, whereas the neutron energy of 3.7 MeV is from the ⁷Li(p, n) reaction at Pelletron facility, TIFR, Mumbai. The ⁶⁴Ni(n, γ) ⁶⁵Ni and ⁵⁸Ni(n, p) ⁵⁸Co reactions cross-sections from present work are compared with the available literature data and found to be in good agreement. The ⁵⁸Ni(n, p) ⁵⁸Co reaction as a function of neutron energy is also calculated theoretically using TALYS computer code version 1.2 and found to be higher than the experimental data.     

Elemental characterisation of strawberry grown in Islamabad by <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript>-instrumental neutron activation analysis and atomic absorption spectrophotometry and its dietary assessment

Mineral contents of strawberry, collected from different farms of Islamabad were analysed by semi-absolute k ₀-instrumental neutron activation analysis and atomic absorption spectrophotometry. The samples were irradiated at two research reactors located in Pakistan Institute of Nuclear Science & Technology (PINSTECH), Islamabad. The analytical methodologies were validated by analysing reference materials, IAEA-336 (lichen) and IAEA-V-10 (hay powder). In all the samples, a total of 26 elements were quantified, among them 16 elements (Ca, Cd, Cl, Co, Cr, Cs, Fe, K, Mg, Mn, Na, Pb, Ru, Sc, Sr and Zn) were found in all the samples. The determined elemental concentrations in strawberry were compared with the reported values from other countries. In comparison with the mineral contents of other fruits, strawberry stands best source of Mn and the second most important source of K after banana. Intake of trace metals through this source was calculated and it was found that strawberry provides Mn (1.95–3.68 mg/kg), Cr (19.2–46.3 × 10⁻³ mg/kg), Fe (3.45–8.72 mg/kg), K (1,520–1,670 mg/kg) and Mg (100–220 mg/kg), which forms 26, 19, 14, 7 and 7% of the recommended dietary allowances for the respective metals. The daily intake of Cd and Pb were compared with the provisional tolerable weekly intake defined by FAO/WHO.     

Thermodynamic investigation of room temperature ionic liquid

The molar heat capacities of the room temperature ionic liquid 1-butyl-3-methylimidazolium hexafluoroborate (BMIPF₆) were measured by an adiabatic calorimeter in temperature range from 80 to 390 K. The dependence of the molar heat capacity on temperature is given as a function of the reduced temperature (X) by polynomial equations, C _P,m (J K⁻¹ mol⁻¹) = 204.75 + 81.421X − 23.828 X ² + 12.044X ³ + 2.5442X ⁴ [X = (T − 132.5)/52.5] for the solid phase (80–185 K), C _P,m (J K⁻¹ mol⁻¹) = 368.99 + 2.4199X + 1.0027X ² + 0.43395X ³ [X = (T − 230)/35] for the glass state (195 − 265 K), and C _P,m (J K⁻¹ mol⁻¹) = 415.01 + 21.992X − 0.24656X ² + 0.57770X ³ [X = (T − 337.5)/52.5] for the liquid phase (285–390 K), respectively. According to the polynomial equations and thermodynamic relationship, the values of thermodynamic function of the BMIPF₆ relative to 298.15 K were calculated in temperature range from 80 to 390 K with an interval of 5 K. The glass transition of BMIPF₆ was measured to be 190.41 K, the enthalpy and entropy of the glass transition were determined to be ΔH _g = 2.853 kJ mol⁻¹ and ΔS _g = 14.98 J K⁻¹ mol⁻¹, respectively. The results showed that the milting point of the BMIPF₆ is 281.83 K, the enthalpy and entropy of phase transition were calculated to be ΔH _m = 20.67 kJ mol⁻¹ and ΔS _m = 73.34 J K⁻¹ mol⁻¹.     

Production of <Superscript>122</Superscript>Sb for the study of environmental pollution

This article presents, ¹²²Sb (T _1/2 = 2.723 days, I _β- = 97.59%) was produced via the ^natSn(p,xn) nuclear process at the AMIRS (Cyclone-30, IBA, Belgium). The electrodeposition experiments were carried out by potassium stannate trihydrate (K₂Sn(OH)₆) and potassium hydroxide. The optimum conditions of the electrodeposition of tin were as follows: 40 g/L ^natSn, 20 g/L KOH, 115 g/L K₂Sn(OH)₆, DC current density of 5 A/dm² with a bath temperature of 75 °C. The electroplated Tin-target was irradiated with 26.5 MeV protons at current of 180 μA for 20 min. Solvent extraction of no-carrier-added ¹²²Sb from irradiated Tin-natural target hydrochloric solution was investigated using di-n-butyl ether (C₈H₁₈O). Yields of about 3.61 MBq/μAh were experimentally obtained.     

Dating of mineral samples through activation analysis of argon

Mass Spectrometry has been the usual method to determine Ar concentrations in mineral samples for dating them through the⁴⁰Ar/⁴⁰K ratio. This technique has been replaced since 1966 by measurement of⁴⁰Ar/³⁹Ar ratio, after artificial production of³⁹Ar from the³⁹K(n,p)³⁹Ar reaction produced in the fast neutron flux of a nuclear reactor. This method requires the fusion of the sample by incremental heating until reaching a temperature of 1000°C in order to get the total release of both argon isotopes. In principle, it should be possible to determine the⁴⁰Ar/⁴⁰K ratio by activation analysis in an easier, non-destructive way, but it presents the following drawbacks: manufacture of argon standards; usual low ratio peak/Compton distribution for both peaks: 1.29 Mev and 1.52 Mev (⁴¹Ar and⁴²K respectively), since potassium minerals are usually very rich in sodium, manganese and chlorine; reaction⁴¹K(n,p)⁴¹Ar induced by fast neutrons present in the thermal flux; and possible contamination of the samples and standards with atmospheric⁴⁰Ar (99.6% of elementary Ar, whose proportion in the atmosphere at sea level is 0.93%). This paper describes how these problems may be solved, also determining the limits of Ar and K concentration related to Compton distribution, in our experimental conditions.     

Magnetic structure and properties of Cu3(OH)4SO4 made of triple chains of spins s=1/2

Cu₃(OH)₄SO₄, obtained by hydrothermal synthesis from copper sulfate and soda in aqueous medium, is isostructural with the corresponding antlerite mineral, orthorhombic, space group Pnma (62), with a=8.289(1) b=6.079(1) and c=12.057(1) Å, V=607.5(2) ų, Z=4. Its crystalline structure has been refined from X-ray single crystal and powder neutron diffraction data at room temperature. It consists of copper (II) triple chains, running in the b-axis direction and connected to each other by sulfate groups. The magnetic structure, solved from powder neutron diffraction data at 1.4 K below the transition at 5 K evidenced by susceptibility and specific measurements, reveals that, inside a triple chain, the magnetic moments of the copper ions (μ_B=0.88(5) at 1.4 K) belonging to outer chains are oriented along the c-axis of the nuclear cell, with ferromagnetic order inside a chain and antiferromagnetic order between the two outer chains. No long-range magnetic order is obtained along the central chain with an idle spin behavior.     

Properties and performance of BaxSr1−xCo0.8Fe0.2O3−δ materials for oxygen transport membranes

The present paper discusses the oxygen transport properties, oxygen stoichiometry, phase stability, and chemical and mechanical stability of the perovskites (BSCF) and (SCF) for air separation applications. The low oxygen conductive brownmillerite phase in SCF is characterized using in-situ neutron diffraction, thermographic analysis and temperature programmed desorption but this phase is not present for BSCF under the conditions studied. Although both materials show oxygen fluxes well above 10 ml/cm²·min at T=1,273 K and pO₂=1 bar for self-supporting, 200 μm-thick membranes, BSCF is preferred as a membrane material due to its phase stability. However, BSCF’s long-term stable performance remains to be confirmed. The deviation from ideal oxygen stoichiometry for both materials is high: δ>0.6. The thermal expansion coefficients of BSCF and SCF are 24×10⁻⁶ and 30×10⁻⁶ K⁻¹, respectively, as determined from neutron diffraction data. The phenomenon of kinetic demixing has been observed at pO₂<10⁻⁵ bar, resulting in roughening of the surface and enrichment with alkaline earth metals. Stress–strain curves were determined and indicated creep behavior that induces undesired ductility at T=1,073 K for SCF. Remedies for mechanical and chemical instabilities are discussed.