Multielement determination in water by instrumental neutron activation analysis

Instrumental neutron activation analysis /INAA/ technique has been applied to a water sample to determine the elemental concentrations. The sample was irradiated with a neutron flux of 1.2×10¹² n cm^–2 s^–1 for two different periods followed by counting at three different decay times, using two coaxial type high-resolution Ge/Li/ detectors. The dominant elements determined in the water sample are Ca, Cl, Na, Mg, and K present in ppm-level while Co, I, Mn, Sm, and Sb are present in smaller amounts, approximately on the average 0.01 ppm. Only traces of other elements such as the rare-earth elements, Ag, As, Ba, Cu, Cd, Fe, Sr, W, Zn, seem to be present in the water sample.     

Activation analysis opportunities using cold neutron beams

Guided beams of cold neutrons being installed at a number of research reactors may become increasingly available for analytical research. A guided cold beam will provide higher neutron fluence rates and lower background interferences than in present facilities. In an optimized facility, fluence rates of 10⁹ n·cm^–2·s^–1 are obtainable. Focusing a large area beam onto a small target will further increase the neutron intensity. In addition, the shift to lower neutron energy increases the effective cross sections. The absence of fast neutrons and gamma rays permits detectors to be placed near the sample without intolerable background, and thus the efficiency for counting prompt gamma rays can be much higher than in present systems. Measurements made at the hydrogen cold source of the FRJ-2 (DIDO) reactor at the KFA provide a numerical evaluation of the improvements in PGAA with respect to signal-to-background ratios of important elements and matrices.     

Trace element determination in high-purity scandium by neutron activation analysis and pre-irradiation matrix separation

A pre-irradiation separation procedure has been developed for the determination of trace elements in high-purity scandium by neutron activation analysis. The sample is dissolved in high-purity concentrated hydrochloric acid and scandium is extracted with the same volume of a solution of 50 vol.% bis(2-ethyl hexyl)-orthophosphoric acid (HDEHP) in toluene. The scandium matrix is removed from the most important trace impurities and the residual amount of Sc is in the range of 0.001%. The separation is carried out in the vial to be used in irradiation to prevent sample contamination. Detection limits in the ppb range were achieved with a sample of 10 mg, a thermal neutron flux of 2 · 10¹³ n · cm^–2 · s^–1 and an irradiation time of 48 hours. Most of the elements sought in two samples of high-purity scandium were below the detection limits.     

Study on air pollution monitoring in Korea using instrumental neutron activation analysis

Trace elements in airborne particulate matter collected monthly at suburban and rural areas in Korea were analyzed by instrumental neutron activation analysis (INAA). Neutron irradiation of the samples was done at the irradiation hole (neutron flux 1·10¹³ n·cm^–2·s^–1) of the TRIGA Mark-III Research Reactor in the Korea Atomic Energy Research Institute. For the verification of the analytical technique, two reference materials, NIST SRM-1648 and NIES CRM-8, were chosen for analysis. The accuracy and precision of the determinations of the 40 elements were compared with the reference values. We used this method (1) to analyze 30 trace elements in airborne particulate matter collected monthly with the high volume air sampler (PM-10) at two different locations and (2) to confirm the possibility of using this method as a routine monitoring tool to find out environmental pollution sources.     

Prompt gamma neutron activation analysis of boron with a 241Am-Be neutron source

A prompt gamma neutron activation analysis (PGAA) setup installed at ANRTC has been used to analyze boron. It consists of a 22.6% REGe detector and a 740 GBq ²⁴¹Am-Be neutron source moderated with water and paraffin. At the sample irradiation position, the thermal neutron fluence rate measured was 2.36·10⁴ n·m^–2· s^–1 and the corresponding Cd-ratio was 22 for gold monitor. The absolute detection efficiency in the range of 120–1500 keV was determined using ¹⁵²Eu standard solution. The sensitivity and detection limit for standard boric acid samples has been determined. The boron content in boric acid prepared from Turkish borate ores is measured to be 15.91±0.46% wt.     

Prompt gamma neutron activation analysis of boron with a 241Am-Be neutron source

A prompt gamma neutron activation analysis (PGAA) setup installed at ANRTC has been used to analyze boron. It consists of a 22.6% REGe detector and a 740 GBq ²⁴¹Am-Be neutron source moderated with water and paraffin. At the sample irradiation position, the thermal neutron fluence rate measured was 2.36·10⁴ n·m^–2· s^–1 and the corresponding Cd-ratio was 22 for gold monitor. The absolute detection efficiency in the range of 120–1500 keV was determined using ¹⁵²Eu standard solution. The sensitivity and detection limit for standard boric acid samples has been determined. The boron content in boric acid prepared from Turkish borate ores is measured to be 15.91±0.46% wt.     

A comparative study of trace elements in water from various sources in surrounding areas of Nagpur city (India) by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) has been used for the determination of 27 elements (Ag, Au, Ba, Br, Ce, Co, Cr, Cs, Eu, Fe, Ga, Hg, Hf, K, La, Mn, Na, Sb, Sc, Se Sr, Th, P, Ta, Tb, Zn and Zr) in 15 water samples collected from different sources (reservoirs, well, borewell, sewage tank, river, rain) in and around Nagpur city (central India) including doubly distilled and a sea water sample from Bombay. Sample residues after evaporation were irradiated at a thermal neutron flux of 10¹²–10¹³ n·cm^–2·s^–1 for 10 min, 1d and 1wk and counted using a HPGe detector and an 4k MCA at different intervals. Several environmental standards from NIST (USA), NIES (Japan) and USGS rock were also analysed for quality assurance. Wide variations in elemental concentrations have been observed in water samples from different sources. Most elemental concentrations in drinking water from various sources, are within ISI/WHO limits. Sea water showed very high concentrations of Ba, Cr, Co, Fe, Hg, Sb, Se and Zn. For doubly distilled and rain waters, however, very low elemental concentrations of Ba, Ce, Fe, Sc, Hg, Se, Sr and Th were observed.     

Measurement of30Si as a tracer by neutron-induced prompt gamma-ray analysis

The application of stable isotope analysis using neutron-induced prompt -ray analysis (PGA) with cold/thermal neutron beams for the tracer study of geological materials are discussed. Silicon has three natural isotopes differing in abundance:²⁸Si (92.23%),²⁹Si (4.67%) and³⁰Si (3.10%). For the purpose of the assessment of Si migration in engineered barrier material, enriched³⁰Si can be used as a tracer due to its nuclear and chemical properties. Isotope analysis of³⁰Si was performed by PGA during the tracer study. Neutron intensity at the sample position was 1.4·10⁸ n¢cm^–2·s^–1, 2.4·10⁷ n·cm^–2·s^–1 for cold and themal neutron guided beams of JRR-3M, respectively. Calibration curves and analytical sensitivity of³⁰Si were determined based on measurement of standard samples. BG and detection limits for³⁰Si analysis were also measured in Japanese bentonite (Kunigel V1 and Kunipia F) and their pore water. Fiffteen elements were determined simultaneously using PGA.     

Analytical possibilities of the BOR 60 reactor

The analytical potential of a fast neutron reactor has been studied. The maximum density of the neutron flux is 2.5·10¹⁵ cm^–2·s^–1 at a maximum energy of 450 keV. The determining reaction for activation analysis at this reactor is an (n, n) reaction. The possibility of selectively determining Pb, Hg, Cd, Au, Ag and other elements at a level of 10^–5–10^–8% is demonstrated. This activation technique allows rapid determination of these elements.     

The validation of a method for determining the migration of trace elements from food packaging materials into food

A new radiotracer method has been developed to measure the migration of trace elements from food contact packaging into four standard food simulants; acetic acid, ethanol, olive oil, deionised water. A sample of material is irradiated in a thermal neutron flux of 10¹⁶n·m^–2·s^–1 to activate the trace elements and produce a range of radionuclides. The sample is then placed in the food simulant and the migration of the radionuclides is monitored by performing -ray spectrometry on a sample of the simulant. Any radionuclides measured must be due entirely to the migration of the elements present in the plastic, since the simulant itself is not radioactive. Preliminary studies have shown that detection limits of around 0.2g·dm^–2 (0.002 mg/kg) can be achieved for antimony in a sample of polyethylene terephthalate. This method can now been extended to measure migration into real foods. This will highlight any differences between the standard simulants currently used and real foods. Since the method only involves irradiation of the packaging material, any food matrix can be studied.     

Neutron activation analysis of low level lithium in water samples

For determining low level lithium concentrations in water, a neutron activation method based on the measurement of tritium radioactivity produced by⁶Li(n,)³H reaction has been developed. This method is specific and free from interference by other chemical elements. Using a low background liquid scintillation counter for tritium measurement, the detection limit is approximately 0.3 ppm during irradiation at a thermal neutron flux density of 1.1·10⁷n·cm^–2·s^–1 for 6 hours by a small nuclear reactor and liquid scintillation counting for 2000 minutes     

Study of the correlation of trace elments in human hair and internal organs by NAA

24 male autopsy cases aged 35–60 years have been collected from Shanghai China to study the relationships between human hair and internal tissues. Autopsy samples of hair, kidney-cortex, liver and lung were analyzed. A radiochemical neutron activation analysis (RNAA) based on a simple group extraction scheme was used for measuring the trace elements As, Cd, Hg, Cu and Zn. Zinc diethyldithiocarbamate Zn(DDC)₂ and methly isobutyl ketone-iodide have been chosen as reagent. Trace element of Se was determined by instrumental neutron activation analysis (INAA). A SLOWPOKE reactor with a thermal neutron flux of 8·10¹¹ n·cm^–2·s^–1 and a swimming pool type reactor with a thermal neutron flux of 1·10¹³ n·cm^–2·s^–1 were used for short and long irradiation of samples, respectively. The reliability of methods has been checked by analyzing biological standard reference materials Horse Kidney (IAEA H8), Tomato Leaves (NBS 1573) and Human Hair (NIES-5). The analytical results show that toxic elements As, Cd and Hg exist in a larger individual variability than the essential elements of Cu, Se and Zn for each tissue. A linear regression analysis related to the six elements of primary interest for the IAEA Coordinated Research Program (CRP) has been done by a computer program for each pair of hair-tissue. A positive correlation is found between concentration of As in hair and kidney-cortex, the correlation coefficient r is 0.751 (p<0.01). Positive correlations between concentration of Se in hair and liver, kidney-cortex and lung are also observed in this study. It shows that the elements As and Se in hair may be useful indicators for assessing certain internal tissues of normal persons. A comparison of Cd concentration in lung shows a significant difference between smokers and non-smokers. A significant correlation between element Cd and Zn in kidney-cortex is also presented in this paper.     

Determination of rare earth elements in phosphorites by neutron activation analysis

Fourty three phosphorite rocks from Western Iraq were analyzed for eleven REE as well as uranium by NAA using IRT Reactor with a neutron flux of 2.3·10¹³ n·cm^–2·s^–1. The gamma activity from each sample was counted with a Ge(Li) and well-type HPGe, each detector connected to an on-line computer. Uranium fission products and different reaction interferences were assessed and allowed for. The results were also checked against international reference materials.     

Characterization of an epithermal irradiation facility

An epithermal energy neutron irradiation facility has been used to perform instrumental activation analysis for iodine, silicon, nickel, zirconium, uranium and thorium. The facility, which is adjacent to the fuel of the University of Virginia 2.0 MW pool reactor, consists of a dry sample region surrounded by a fixed cadmium shield. A boron nitride capsule can be used to hold the sample in the cadmium facility to further enhance the reduction of thermal neutron activation. The neutron fluence rate is 2.2×10¹⁶ n·m^–2·s^–1 for fission spectrum energy neutrons (measured with Ni(n,p)Co) and 8.2·10¹⁵ n·m^–2·s^–1 for resonance energy neutrons (measured with gold).Iodine has been measured at concentrations as low as 0.1 mg/kg with 3% counting statistics in powdered infant formula and 0.15 mg/kg with 5% statistics in liquid infant formula. Silicon has been measured at concentrations of 0.2% in biological samples with counting statistics between 5 and 10% and in coal and soil at concentrations greater than 4% with better than 1% statistics. Nickel has been measured in coal and soil at the 20 mg/kg level and higher with 6% statistics. Zirconium has been determined at 600 mg/kg and greater in ceramics with counting errors less than 3%. Uranium and thorium have been measured at the 10 mg/kg level with 3% counting statistics.     

Separation of fluoride ion by extraction with triphenyltin chloride. Application for NAA of fluorine by means of 14-MeV neutrons

The separation of fluoride by extraction with toluene solution of triphenyltin chloride has been studied. Quantitative isolation of fluoride from solutions with a wide acidity range (pH 4.0–11.5) has been established. It is suggested that interferences by Ca, Mg, Fe, and Al can be avoided by masking these elements using sulfate and hydroxyde ions. Interference by phosphate ions can be overcome in a similar fashion. The halogenated species can be masked by mercury nitrate. Detection limit for fluorine determination is about 3 g for a neutron generator flux of 2·11¹¹ n·cm^–1·s^–1. A method for fluorine assay in water using a neutron generator with a detection limit of 1 ppm has been developed.     

Weight loss as error source in neutron activation analysis of biological samples

Summary Neutron activation analysis (NAA) is a useful method to determine the concentration of trace elements in biological samples. But it has its special problems and error sources. An extensive study was performed to prove that weight loss affects both accuracy and precision of NAA based on post-irradiation weights. Weight losses of 5 ± 3% and 14 ± 7% (mean ± SD) were observed after irradiating blood and its main components for more than 12 h with thermal neutron fluxes of about 10¹⁴n · cm^–2 · s^–1 in two reactors with different cooling facilities. These losses were flux-dependent, but independent of irradiation time, sample donor, type and size, and post-irradiation time and handling. In order to avoid this NAA-specific error elemental concentrations should be based on pre-irradiation weights.

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Gewichtsverlust als Fehlerquelle bei der Neutronenaktivierungsanalyse biologischer Proben

     

A search for losses of chemical elements during freeze-drying of biological materials

Possible losses of seven chemical elements were investigated in biological tissues during freeze-drying in vacuum. Thyroid glands were taken during post-mortem examination of 23 people died of different diseases. Instrumental neutron activation analysis (INAA) was used to estimate contents of Br, Ca, Cl, I, K, Mg, and Na. The nuclear reator vertical channel with flux density of 1.2·10¹³n·cm^–2·s^–1 was used for neutron irradiation. The analysis was carried out using short-lived radionuclides induced in samples after neutron irradiation. Then thyroids were freeze-dried at below 0 °C in vaccum up to the constant mass (lyophilisation) and then homogenized. Samples of lyophilised and homogenized tissues were again studied by INAA. The lack of difference between the results of the analysis before and after lyophilisation is an evedence of no loss of Br, Ca, Cl, I, K, Mg and Na during freeze-drying of biotissues in vaccum.     

Determination of trace elements in Nigerian kola-nuts by instrumental neutron activation analysis

The trace elements content of Cola acuminata and three varieties of Cola nitida have been determined using neutron activation analysis. The samples have been irradiated at the Joint Universities Research Reactor, Risley, England for 7^1/2 hours in a neutron flux of 2.5·10¹² n·cm^–2s^–1 and analysed using high resolution lithium drifted germanium detector coupled to a Canberra 35 microprocessor as a 4096 channel gamma spectrometer. The elements: Na, K, Br, W, Fe, Cs, Co, Zn, and Sc were detected.     

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.     

Intercomparison and determination of environmental standard samples by instrumental neutron activation analysis

To identify and improve the analytical technique for air pollution research, four kinds of environmental standard samples, i.e., airbome particulate matter, coal flyash, soil and pine needle supplied from the NIST and the IAEA were analyzed using thermal and epithermal neutron activation techniques. Sample irradiation was done at the irradiation facilities (neutron flux, 1 · 10¹³ n·cm^–2·s^–1) of the TRIGA MARK-III Research Reactor in the Korea Atomic Energy Research Institute. The accuracy and precision for the analysis of 40 trace and toxic elements in the samples were compared with the certified and reported values, respectively. In the analytical results of all standard reference materials, the relative standard deviation were within the 15% except for 11 elements and the relative error were agreed within the 10–20% except for 13 elements. The benefit of epithermal activation was investigated and the optimum analytical condition is reported.