Estimation of sulfur in coal by fast neutron activation

A simple method is described for estimation of sulfur in coal using fast neutron activation of sulfur, i.e.³²S(n,p)³²P and subsequent measurement of³²P -activity (1.72 MeV) by a Geiger-Müller counter. Since the sulfur content of Indian coal ranges from 0.25 to 3%, simulated samples of coal containing sulfur in the range from 0.25 to 3% and common impurities like oxides of aluminium, calcium, iron and silicon have been used to establish the method.     

Elemental analysis of fertilizer by fast neutron activation

A simple and accurate technique has been developed to analyse the commercial fertilizers for phosphorous, potassium, chlorine, magnesium and silicon. The method is based on the fast neutron activation.     

Protein determination in soya bean by fast neutron activation analysis

For a non-destructive determination of the protein content in soya bean samples, 14-MeV neutron activation analysis /NAA/ was applied. To check the method, results obtained by X-ray fluorescence /XRF/ analysis and the Kjeldahl procedure were compared. For pressed pellet samples of about 1 g and choosing 15 min irradiation and 10 min measuring times the accuracy of the protein determination was found to be 15%.This work was supported by the Hungarian Research Foundation /Contract No. 259/.     

Nitrogen determination in plant samples by fast neutron activation analysis

For the non-destructive deermination of the nitrogen content in plant samples 14-MeV neutron activation analysis was applied. Using powder samples of 0.7 g, irradiation time of 1 h and measuring time of 10 min, the accuracy of the determination is about +15%. The potassium content of the plant samples was determined by X-ray fluorescence analysis and correction was made for their contribution to the nitrogen activities.This work was supported in part by the Hungarian Academy of Sciences.     

Multielement content of coal by neutron activation analysis techniques

Due to the interaction with components present in natural waters, radionuclides may be present in different physico-chemical forms, varying in size, charge and density. The distribution pattern will influence the transport, mobility and biological uptake of the radionuclides. Size fractionation based on hollow fiber is useful for the determination of the size distribution pattern of radionuclides in natural waters. Furthermore, a continuous mixing and separation system has been developed for the investigation of the association of radionuclides with naturally occurring colloids. Results based on radionuclides in waste water from the Forsmark nuclear power plant, Sweden, will illustrate the potential usefulness of the technique.     

Determination of cadmium in environmental materials by fast neutron activation analysis

Cadmium is determined by activation analysis with fast neutrons, obtained by irradiation of a thick beryllium target with 14.5-MeV deutrons. Cadmium-111m, formed via the ¹¹²Cd(n, 2n)^111mCd and ¹¹¹Cd(n, n′)^111mCd reactions, is separated by liquid—liquid extraction with zinc dithyldithiocarbamate in chloroform and measured with a Ge(Li) γ-spectrometer. For low concentrations, cadmium is precipitated as cadmium ammonium phosphate after the extraction. NBS and BCR reference materials were analyzed: for concentrations between 3 and 500 μg g^?1, the relative standard deviation ranges from 5 to 3% The results obtained for sewage sludge are compared with those obtained by reactor neutron activation analysis.     

The determination of fluorine in bone by fast neutron activation analysis

A routine method is presented for the determination of fluorine in small bone samples by activation analysis with fast conversion neutrons. Both the purely instrumental determination and the analysis by chemical separation are discussed. The activations are performed with the AVF cyclotron of Philips-Duphar at Petten. Use was made of a rabbit system equipped with a Be-target, which can be inserted in the internally deflected beam of the cyclotron. The sensitivity of the instrumental method is ≈1 μg. Application of chemical isolation results in a sensitivity of ≈0.1 μg.     

Oxygen and nitrogen in coal by instrumental neutron activation analysis

The feasibility of using fast neutron (14 MeV) activation analysis techniques for the determination of oxygen and nitrogen in coal has been investigated. Conditions that favor instrumental neutron activation analysis (INAA) include the absence of problems associated with sample dissolution and the capability of extremely rapid analyses as compared to older techniques such as the Kjeldahl method for nitrogen. Most previous oxygen determinations have been by difference after major component analyses. In the present study, oxygen was determined in sized coal and its low temperature ash (LTA) with the difference representing the organic oxygen content. Both the oxygen and nitrogen analyses employ a multiscaling technique with the former based on the¹⁶O(n, p)¹⁶N reaction, while the latter utilizes the annihilation radiation produced by the product of the¹⁴N(n, 2n)¹³N reaction. The high-energy gamma-radiation associated with the decay of¹⁶N was essentially free of spectral interferences for coal analysis, although fluorine could cause a primary interference if the F/O ratio exceeds 0.02. In the nitrogen work, experiments were performed to determine correction factors to account for the effects of the¹²C(p, γ)¹³N and¹³C(p, n)¹³N “knock-on” reactions and the³⁹K(n, 2n)³⁸K reaction which produce interfering β⁺ emitting radionuclides. Data are presented for oxygen in Western Kentucky No. 9 and No. 11 coal and coal ash and for nitrogen in eleven different coals.     

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.     

Oxygen determination by fast neutron activation

A method for the determination of oxygen based on the reaction¹⁶O(n, p)¹⁶N is suggested. The samples are irradiated in stainless steel capsules with fast neutrons. The total neutron flux passing through the sample is proportional to the flux passing through the wall of the capsule. Therefore, the activity induced in the capsule according to the reaction⁵⁶Fe(n, p)⁵⁶Mn can be used to monitor the neutron flux through the sample. Thus, the necessity of maintaining the sample in an exact position during the irradiation is eliminated.     

Gamma-ray tables for neutron fast neutron and photon activation analysis

In the past several years, a number of gamma-ray tables have been published. All of the tables limit themselves to those nuclides formed in (n, γ) reactions or at most to a few of the more prominent (n, 2n) products. A number of investigators are developing activation analysis methods using fast neutrons or photons. These investigations have been hampered by the lack of tables of gamma-rays of those nuclides that can be formed by (n, 2n), (n, p), (n, α), (n, n′) and (n, d) reactions. Since (γ, n) yields the same product as (n, 2n) the table would also be useful to photon activation studies. The authors have compiled such a table. Section II: list of the gamma-rays for all isotopes in order of increasing energy will be published in the J. Radioanal. Chem., 25 (1975) No. 2.     

Determination of aluminium in bulk coal samples by neutron activation analysis

The determination of Al₂O₃, in bulk coal samples to an accuracy of about 0.2% Al₂O₃ has been achieved by means of a thermal-neutron activation technique based on the reaction ²⁷Al(n,γ)²⁸Al. In the analysed samples, which had widely different compositions, the Al₂O₃ concentrations ranged from 1 to 11% and the ash contents from 7 to 40%. Al₂O₃ concentrations measured by x-ray fluorescence showed a linear relationship with both the 1.78-MeV γ-ray count following the decay of ²⁸Al and the thermal-neutron count near the samples during irradiation. The linear relationship, which was obtained by regression analysis of the experimental data, determined the Al₂O₃concentrations with a standard deviation of 0.24% Al₂O₃. The particle sizes in the samples ranged from —0.5 to —40 mm, the moisture contents ranged from 1 to 6%, and the sample weights ranged from 8 to 11 kg. However, inclusion of these parameters in the regression analysis did not significantly improve the results for Al₂O₃.     

Estimation of rubidium in coconut palm leaves by neutron activation analysis

A simple and rapid method is described for the estimation of the rubidium in coconut palm leaves by neutron activation analysis. The method is found suitable for the estimation of stable Rb used as a tracer in root distribution studies. The average of five determinations is 5.15 μg, which varies between 5.07 μg and 5.26 μg at 95% confidence limit.     

Updating analytical techniques for fast neutron activation analysis

Two improvements in the analytical techniques used for fast neutron activation analysis have been developed and put into routine use. The first is neutron shielding of a NaI (TL) counting system, which reduces the counting noise encountered during neutron generation. The second is a modification of batch type irradiation for long lived nuclides so they can be done simultaneously with other test.     

Trace elemental composition of Nigerian coal measured by neutron activation analysis

The instrumental neutron activation analysis (INAA) technique has been used to determine 17 major, minor, and trace elements in samples of the three major sources of Nigerian coal. The NBS Standard Reference Material, Coal SRM 1632, was also analyzed, for the purpose of verifying the accuracy of the method. The results obtained with it were in good agreement with the NBS certified values. The concentrations of the major elements determined for the Nigerian coal were found to be much lower than the mean values of those reported for coal samples from other parts of the world.     

The multielement potential of fast neutron cyclic activation analysis

Cyclic neutron activation analysis (CNAA), has, in recent years been developed as a useful analytical tool for the assay of short-lived isotopes in single element situations. The work described in this paper investigates the potential of the technique for composite samples having a wide range of elements that produce short-lived and long-lived isotopes on neutron irradiation. Accelerator-derived neutrons with average energies of 3 MeV, 6MeV and 14MeV were employed in what has been dubbed Fast Neutron Cyclic Neutron Activation Analysis (FNCAA). The approach to multi-element analysis entailed: (a) determination of cycle parameters in single element samples via the reactions²⁷Al(n, p)²⁷Mg (9.6 min,E =840keV), and¹³⁷Ba(n, n)^137mBa(2.3min,E =662keV), (b) a test of the method on a composite rock sample, (c) determination of analytical sensitivities using both powdered kale and rock standards and (d) a comparison of analytical results with other techniques. The results obtained in all these measurements are presented and discussed.     

Determination of sulfur in steels by radiochemical neutron activation analysis with liquid scintillation counting

A method has been developed for the determination of low-level sulfur in steels by radiochemical neutron activation analysis. During sample irradiation, ³⁵S is produced by the ³⁴S(n,γ)³⁵S reaction. Irradiated steels are mixed with sulfur carrier and dissolved in HCl/HNO₃. Sulfur is reduced to H₂S by reaction with HI/H₃PO₂/HCl. The evolved H₂S is absorbed in dilute NaOH, which is mixed with scintillation cocktail for the measurement of ³⁵S by liquid scintillation counting. Sulfur carrier yield is determined by iodometric titration. Chlorine is also determined by RNAA in order to correct for ³⁵S produced via the ³⁵Cl(n,p)³⁵S reaction. Sulfur has been determined at mass fractions as low as ≈5 mg/kg in ultra-high-purity iron using this method.     

Possibilities of the elemental analysis of dry biological material by fast neutron activation analysis

The applicability of a 400 kV neutron generator in the elemental analysis of dry biological material is considered. Data for the specific count-rates of 66 elements are given. A procedure for the determination of N, Mg, Si, P, K and Ca is described. The results for three Standard Reference Materials and some samples are given.     

Determination of silicon,phosphorus and sulfur in alloy steel by neutron activation analysis

Silicon, phosphorus, and sulfur in alloy steel were determined by neutron activation analysis involving rapid radiochemical separation procedures. The standard deviations for silicon, phosphorus, and sulfur were 1.6%, 2.3%, and 2.4% respectively; the sensitivity limits were 3.2, 0.20, and 2.50 p.p.m., respectively. The three constituents could be determined in alloy steel within 2 h of the irradiation.     

Accurate fast neutron activation analysis for oxygen in geological materials

Sources of error in the fast neutron activation analysis determination of oxygen have been investigated and minimised. The oxygen contents of eighteen international rock standards and a sulphide ore standard have been determined, and compared with the values calculated by difference using the reported full analyses. Accuracies of 0.3% average deviation and reproducibilities of ±0.2% standard deviation have been obtained, where oxygen contents exceeded 1.0 g.