Substoichiometric determination of manganese by neutron-activation analysis

A simple and rapid method for the substoichiometric determination of traces of manganese in various materials by neutron-activation analysis has been developed. After dissolution of the irradiated test sample, manganese(II) carrier is added and subsequently oxidised by peroxodisulphate to the heptavalent state. The permanganate thus formed is finally extracted into chloroform as tetraphenylarsonium permanganate using a substoichiometric amount of tetraphenylarsonium chloride. This single separation step isolates radiochemically pure manganese-56 in the analysis of a relatively simple material in which interfering elements (gold, rhenium, etc.) are absent. When this is not true, a preliminary separation of manganese from the irradiated sample, based on the extraction of manganese diethyldithio-carbamate into chloroform and followed by stripping of the manganese with dilute sulphuric acid, must be used. A simultaneously irradiated standard containing manganese must be treated in exactly the same way as a test sample. In the materials analysed by the new method 10(-5) to 10(-3)% of manganese has been determined.     

Photon-activation analysis for carbon and oxygen

A method is described for the determination of carbon and oxygen in organic materials by means of the reactions (12)C(gamma, n)(11)C and (16)O(gamma, n)(15)O. Samples are irradiated with bremsstrahlung from a 32-MeV electron beam impinging on a tungsten target, and the active products are separated before the positron annihilation gamma rays are counted. Limits of detection of 0.003 mug of carbon and 0.1 mug of oxygen are obtained.     

Determination of manganese in ores by activation analysis using a californium-252 neutron source

A²⁵²Cf neutron source has been used to analyse manganese in ores such as pyrolusite, rodonite (manganese silicate) and blends used in dry-batteries. Samples with about 150 mg and standards of manganese dioxide were irradiated for about 20 min and counted using a well-type NaI(Tl) scintillation counter and scaler, with or without pulse-height discriminator between the detector and the scaler. The interferences of nuclear reactions⁵⁶Fe(n,p)⁵⁶Mn and⁵⁹Co(n,α)⁵⁶Mn were studied, as well as problems in connection with neutron shadowing during irradiation, gamma-rays attenuation during counting and influence of granulometry of samples. Some of the samples were also analysed by wet-chemical method (sodium bismuthate) in order to compare results.     

Gamma irradiation increases the antioxidant properties of Tualang honey stored under different conditions

This study was conducted to evaluate the effects of evaporation, gamma irradiation and temperature on the total polyphenols, flavonoids and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical-scavenging activities of Tualang honey samples (n = 14) following storage over three, six or twelve months. The mean polyphenol concentrations of the six gamma irradiated honey samples at three, six and twelve months, respectively, were 96.13%, 98.01% and 102.03% higher than the corresponding values of the eight non-gamma irradiated samples. Similarly, the mean values for flavonoids at three, six and twelve months were 111.52%, 114.81% and 110.04% higher, respectively, for the gamma irradiated samples. The mean values for DPPH radical-scavenging activities at three, six and twelve months were also 67.09%, 65.26% and 44.65% higher, respectively, for the gamma irradiated samples. These data indicate that all gamma irradiated honey samples had higher antioxidant potential following gamma irradiation, while evaporation and temperature had minor effects on antioxidant potential.     

Development of a new flow-through bulk optode for the determination of manganese(III)

A flow-through bulk optode based on the use of 1-(2-pyridylazo)-2-naphthol (PAN) immobilized in a plasticized poly(vinyl chloride) membrane entrapped in a cellulose support, in conjuntion with the flow injection analysis technique, is proposed for the determination of manganese(II). The calibration graph obtained at 570 nm was linear in the range 0.27-27.5 mg L(-1) (5 x 10(-6)-5 x 10(-4) M) Mn(II) with a detection limit of 0.18 mg L(-1). The coefficients of variation of the sensor response for 5.5 mg L(-1) of Mn(II) were +/-0.22% for consecutive measurements (n = 10), +/-0.48% between days (n = 5) and +/-0.38% between different membranes (n = 6). The sensor was readily regenerated with the carrier acetic acid/acetate buffer of pH 4.5. The method was applied to the determination of manganese in steels, waters and lemon tree leaves.     

Determination of sodium in high purity silica by activation analysis

High purity fused silica samples and NBS standards were irradiated in the Sandia Reactor Facility for 2 hr at a thermal flux of 10(10) neutrons/cm(2)/sec. (24)Na was produced by the reaction (23)Na(n, gamma)(24)Na (14.9 hr half-life, alpha = 0.5 barn), and decayed with emission of 1.37 and 2.75 MeV gamma-rays. With the stated flux and irradiation time, sodium at the 3 ppm level has been determined with a standard deviation of 0.2 ppm. Values obtained by thermal neutron-activation analysis agree well with results obtained by emission spectrography and flame spectrophotometric methods.     

Induction and detection of radioactivity in foodstuffs irradiated with 10 MeV electrons and X-rays

Induction of radioactivity by direct (γn) and indirect (nγ) means was measured in solutions and foods irradiated with 10 MeV electrons and X-rays, to a dose of 20 kGy. Both types of reaction occur to a very limited extent following electron irradiation and this is attributed to the low efficiency of bremsstrahlung production in the target. For X-rays below the 1981 JECFI recommended 5 MeV upper limit of energy, only four (γn) reactions are possible and all have stable products. However, the neutrons generated can undergo moderation and capture by a variety of nuclides. Of particular interest is the reaction ²H(γn)¹H since this has an abnormally low (γn) threshold of 2.2 MeV and deuterium occurs with a natural abundance of 0.015%; hence some neutron production in food is inevitable. A neutron flux of 1.79 × 10⁵ [n cm⁻² s⁻¹] [μg(D) cm⁻³]⁻¹[kGy s⁻¹]⁻¹ was estimated from the activity induced in a variety of neutron monitors, especially manganese−55, as measured by gamma spectrometry and Cerenkov techniques. Induced activities at the end of irradiation calculated for beef using this flux value total 90 Bq kg⁻¹ which is of the same order as natural levels in food (approx. 100 Bq kg⁻¹), and are in broad agreement with NRPB data.     

Sulfur determination in coal by 14 MeV neutron activation analysis

A procedure involving the irradiation of coal samples with 14 MeV neutrons and subsequent gamma-ray spectrometry of the irradiated sample for the estimation of solfur in coal, has been outlined. The samples were irradiated with 14MeV neutrons from a Cockroft-Walton type generator for one minute and then subjected to gamma-ray spectrometry for another minute using an automated transfer cyclic system. Ten such cycles were repeated for accumulating events under the 2130 keV gamma ray photopeak belonging to³⁴P (T=12.4 s) produced by the³⁴S(n, p)³⁴P reaction for assessing the lower level of detection, LLD, of Sulfur. Interferences due to the presence of other elements in coal were also determined. Sulfur can be determined at LLD of 0.25% in coal provided a 5 g sample of the coal is irradiated with a neutron flux of 5·10⁹ n·cm⁻²·sec⁻¹ assayed with a gamma ray spectrometer having a large hollow core Ge(Li) detector and an anti-Compton shield.     

An application of the monostandard epithermal neutron activation technique for the analysis of domestic phosphate ores

The trace elements As, Co, Eu, Ga, La, Sb, Sc, Sm, U and W and the major constituents Fe and Na were determined in four domestic phosphate rocks by the monostandard epithermal neutron activation technique. Samples of 0.1 g were irradiated in the Egyptian 2 MW ERR-1 reactor under Cd cover, and the induced gamma activities measured after 6 h, 7 d and 8 w with a Hp Ge detector coupled to a computerized multichannel analyzer. Uranium has been used as a monostandard due to its relatively high resonance integral value (I₀=274.6 b) and because it is one of the elements to be determined more accurately. The present data are compared with those obtained by instrumental neutron activation analysis (INAA) method performed at Institute of Radiochemistry, Karlsruhe. The observed discrepancies do not exceed 12% in average. The present method is a practical alternative for trace element analysis.     

Improving accuracy in routine instrumental activation analysis

An INAA procedure for routine analysis of rock samples is described. Samples are irradiated using a rotating sample holder. Measurement of the induced gamma activity is performed using an automatic gamma spectrometer and the elemental concentrations are calculated by a computer. The analytical error is discussed and the precision and accuracy evaluated experimentally. An average error of ±3–5% without considering counting statistics is obtained. Results for 19 elements in 8 international standard rocks are reported. A short discussion of the cost of the analysis is included.     

Comparison of irradiation effects of electrons and gamma rays on PVC samples

Samples of polyvinyl chloride (PVC) were irradiated at a dose of 15 MGy using both electrons and gamma rays. The resultant material shows differences attributed to the very different dose rates in each type of radiation. In addition, a method useful in separating the highly cross-linked portion of the sample has been tested. Transmission electron microscopy, electron stimulated desorption and energy dispersive spectroscopy have been applied in the characterization of the irradiated material. We show that this resultant material, after irradiation, consists mainly of carbon-like material with distinct crystallographic phases which, in some cases, resemble graphitic structures.     

Application of INAA for phyto-accumulation study of selenium by chickpea plant

The phyto-accumulation efficacy of selenium (Se) from soil by chickpea plant is reported. Chickpea plants were grown in soil having different concentrations (1–4 mg kg^?1) of Se. Samples of soil and different parts of chickpea plants in Se rich soil were analyzed for determination of Se concentrations by instrumental neutron activation analysis (INAA). Samples were irradiated in self-serve facility of CIRUS reactor, BARC, Mumbai at a neutron flux of the order of 10¹³ cm^?2 s^?1. The gamma activity at 264.7 keV of ⁷⁵Se (119.8 d) was measured using a 45% relative efficiency HPGe detector coupled to MCA. Dependence of Se distribution in soil and plants on its spiking concentration was evaluated in this work. The Se concentrations determined in plant parts grown in control soil and in soil spiked with Se (4 mg kg^?1) are in the range of 0.6–0.8 and 65–68 mg kg^?1 respectively.     

Determination of phosphorus in polymers by INAA

An INAA technique employing beta spectrometry was developed for the determination of phosphorus in polymers. The (n,γ) reaction on phosphorus produces³²P, half-life 14.3 days, a pure beta emitter with end-point energy 1.71 MeV. Polymer samples in the form of powders, films and pellets are irradiated and then counted with a plastic scintillator. The beta spectrum is corrected for interferences (especially Sb, Zn and Br which are quantified by gamma spectrometry) and for energy loss in the thick sample. Samples must also be analyzed for S and Cl which cause nuclear interferences. With an irradiation time of 4 hours at a neutron flux of 5·10¹¹ n·cm^{−2 s −1}, decay time 10 days and counting time 10 minutes, the sensitivity is 520 counts/μg phosphorus and the detection limit is typically 2μg/g.     

Preparation of radio-Sm by neutron activation for accelerator mass spectrometry

Field measurement of isotopic ratios may be used to fingerprint an element’s origin, be it from commercial power, industrial, medical or historical weapons fallout. Samples of samarium radionuclides were prepared by neutron activation for subsequent analysis using accelerator mass spectrometry (AMS). High purity samarium (III) oxide powder was irradiated in the University of Texas at Austin TRIGA reactor to a total neutron fluence of 5 × 10¹⁵ cm^?2. An initial determination of the isotopic ratios was made using activation calculations with a BURN card in an MCNPX-based model of the TRIGA core. Experimental validation of the MCNP results was achieved by analyzing gamma spectra of the irradiated oxide powers after irradiation. Subsequent measurement of ¹⁵¹Sm will be conducted at the CAMS facility at LLNL demonstrating the first measurement of this isotope at this facility.     

Residual radioactivity measurement for high purity silicon irradiated by pile-neutron (author's transl)

Residual radioactivity measurement is described for high purity silicon (purer than tennine) irradiated by pile-neutron to produce n-type silicon semiconductor. The silicon samples were irradiated in four different atomic reactors with thermal neutron fluxes of 0.12, 1.48, 1.8 and 5.5 X 10(13) n/cm2. sec. After irradiation, the sample was dissolved in HF-HNO3, and the solution dried. The residual radioactivity was measured by a 2pi gas-flow low background GM counter. The only active species found was 32P, which was formed by the consecutive reaction of 30Si(n, gamma)31Si beta- leads to 31P followed by 31P(N, GAMMA)32P. The observed production rate for 32P was in good agreement with the calculated one. This technique can be applied to estimate amounts of not only doped phosphorus but impurities such as gold in irradiated silicon. Tail part of a float-zone silicon rod contained about 0.01 atomic ppb of Au, but no activity was observed in its middle part. The present technique is suitable for checking and characterizing silicon rods before their neutron-doping.     

Spectrophotometric determination of manganese by using redox reaction of tris(2,2'-bipyridine)osmium(II) with Mn7+.

This paper reports on the analytical application of the oxidation reaction of [Os(bpy)3]2+ by Mn7+ (MnO4-). The present study developed a very simple, sensitive and selective spectrophotometric method for the determination of manganese in an acidic medium. Three analytical wavelengths were employed in the UV and visible regions at 290, 315 and 480 nm. Beer's law was obeyed up to a concentration of 330 ng ml(-1) of Mn7+ at different wavelengths with regression equations 0.001 - 0.0042C(Mn), 0.001 + 0.0021C(Mn), and 0.001 - 9.34 x 10(-4)C(Mn) at 290, 315 and 480 nm, respectively. Under the optimum conditions, the achieved detection limits were 0.72, 1.37 and 3.32 ng ml(-1) at 290, 315, and 480 nm, respectively. In addition to the high sensitivity of the method (0.24 ng cm(-2) at 290 nm, 0.45 ng cm(-2) at 315 nm and 1.0 ng cm(-2) at 480 nm), it can be used for the determination of manganese in the presence of a large number of anions and cations, since it tolerates most of the potential interferents. The relative standard deviation was 0.5% (n = 11) for 90 ng ml(-1) manganese. The method was successfully applied to the determination of manganese in water from different resources.     

The effect of gamma irradiation on mechanical, and thermal properties of recycling polyethylene terephthalate and low density polyethylene (R-PET/LDPE) blend compatibilized by ethylene vinyl acetate (EVA)

A study has been made on the compatibility of recycled polyethylene terephthalate (R-PET) and low density polyethylene (LDPE) blend in the presence of ethylene vinyl acetate (EVA) as a compatibilizing agent prepared by extrusion hot stretching process. EVA content in the blend as a compatibilizing agent was an enhancement effect on radiation crosslinking of R-PET/EVA/LDPE blends and the highest radiation crosslinking was obtained when the EVA content was reached at 10 % EVA when irradiated by gamma irradiation. Blends containing different (EVA) ratios were irradiated to different doses of gamma irradiation 25, 50 and 100 kGy. The effect of the compatibilizer and radiation on mechanical, thermal properties of R-PET together with LDPE and morphology has been investigated. It was found that gamma irradiation together with the presence of compatibilizing agent (EVA) has positive effect on the mechanical and thermal properties of R-PET/LDPE blend. The structural properties of R-PET/LDPE modified by gamma irradiation and EVA as compatibilizing agent was examined by SEM. Also, it was found that the optimum concentration of EVA and gamma irradiation dose was found to be 10 % EVA and 100 kGy, respectively.     

Influence of Gamma Radiation on Electrical Conduction of Polyethylene Terephthalate (PET) at Ambient Temperature

The electrical conduction in polyethylene terephthalate (PET) exposed to a gamma radiation dose of 150 kGy was investigated in the applied field range from 4 to 36 kV/mm. Samples were irradiated in air at room temperature by means of a ⁶⁰Co gamma source at a dose rate of approximately 42 Gy/min. The electrical properties of virgin and irradiated materials were examined by charging and discharging current measurements. The current decays with time can be represented according to an inverse power law. The changes of dielectric behavior after irradiation were attributed to scission effects.     

Simultaneous determination of manganese and selenium in serum by electrothermal atomic absorption spectrometry

A method for determination of manganese and selenium in serum by simultaneous atomic absorption spectrometry (SIMAAS) is proposed. The samples (30 mul) were diluted (1+3) to 1.0% v/v HNO(3)+0.10% w/v Triton X-100 directly in the autosampler cups. A total of 20 mug Pd+10 mug Mg(NO(3))(2) was used as chemical modifier. The pyrolysis and atomization temperatures for the simultaneous heating program were 1200 and 2300 degrees C, respectively. The addition of an oxidant mixture (15% w/w H(2)O(2)+1.0% v/v HNO(3)) and the inclusion of a low temperature pyrolysis step (400 degrees C) attenuated the build-up of carbonaceous residues onto the integrated platform. An aliquot of 15 mul of the reference or sample solution was introduced into the graphite tube and heated at 80 degrees C; subsequently, 10 mul of oxidant mixture+10 mul of chemical modifier was introduced over that aliquot and the remaining heating program steps were executed. This strategy allowed at least 250 heating cycles for each THGA tube without analytical signal deterioration. The characteristic masses for manganese (6 pg) and selenium (46 pg) were estimated from the analytical curves. The detection limits were 6.5 pg (n=20, 3delta) for manganese and 50 pg (n=20, 3delta) for selenium. The reliability of the entire procedure was checked with the analysis of serum from Seronormtrade mark Trace Elements in Serum (Sero AS) and by addition and recovery tests (97+/-9% for manganese and 96+/-7% for selenium) using five serum samples.     

Investigation of Organic-Inorganic Hybrid Materials Prepared by Irradiation

New silica-based hybrid materials have been produced by gamma irradiation of the precursors using a ⁶⁰Co source. An inorganic mixture of tetraethylorthosilicate with addition of Zirconium propoxide (PrZr) (x = 0, 5 and 10 mol%) was used together with polydimethylsiloxane (PDMS) silanol terminated. Samples with volume ratios organic/inorganic of 4/1, 3/2, 1/1, 2/3 and 1/4 were prepared. The irradiation dose for gel point was observed to depend on the PDMS/ INORG. volume ratio, as expected. That dose increases with decreasing volume ratio. Samples with PDMS/ INORG = 2/3 were irradiated to several irradiation doses above that corresponding to the gel point, which becomes higher for higher fraction of PrZr added. The resulting samples are homogeneous, transparent and flexible being able of swelling in a good solvent of the polymer. The microstructure of the samples was investigated by Small Angle Neutron Scattering. Samples were measured as prepared, and immersed in deuterated cyclohexane. Results indicate the presence of oxide dense clusters interconnected by polymer structures. The addition of PrZr in the preparation stage increases the density of the clusters and decreases their size.