Neutron activation analysis calibration methods

Selected ion monitoring can be used for the determination of the relative amount of each component of a mixture, introduced into the mass spectrometer by the direct inlet probe However, such a determination requires reference mixtures of known composition for calibration. In the present experiment, since the monochloro pentaziridino derivative had not yet been isolated in the pure form, it was necessary to determine its concentration, by an auxiliary method, in a sample which could then be utilized as a reference mixture for further experiments. In order to do this we titrated chlorine in the toxic sample of MYKO 63 (B) by the classical method. The results indicated that the amount of N3P3AZJCI was between 0.5-1.5 %. The large statistical error is due to the low chlorine content in the sample examined. Thus, we used the remarkable possibilities provided by neutron activation analysis when the impurity to be quantified is a chlorinated moiety. It is well-known indeed that the C1 -f 2n peak is amongst the most easily detectable by neutron... 

Cadmium in acidified aqueous solution may be analyzed at trace levels by various instrumental techniques such as flame and furnace atomic absorption, and ICP emission spectrophotometry. Cadmium in solid matrices is extracted into aqueous phase by digestion with nitric acid prior to analysis. A much lower detection level may be obtained by ICP-mass spectrometry. Other instrumental techniques to analyze this metal include neutron activation analysis and anodic stripping voltammetry. Cadmium also may be measured in aqueous matrices by colorimetry. Cadmium ions react with dithizone to form a pink-red color that can be extracted with chloroform. The absorbance of the solution is measured by a spectrophotometer and the concentration is determined from a standard calibration curve (APHA, AWWA and WEF. 1999. Standard Methods for the Examination of Water and Wastewater, 20th ed. Washington, DC American Public Health Association). The metal in the solid phase may be determined nondestructively by x-ray fluorescence or diffraction techniques. 

FT-IR has been used to determine residual catalyst support in commercial polyethylene at the level of 100 parts per million 841. The method is based on the use of the 1118 or 470 cm-1 bands to determine the quantity of silica support dispersed in the polymer. The band at 2020 cm-1 was used as an internal standard for the amount of polyethylene. Neutron activation analysis was used to calibrate the weight percent of silica present in each polymer sample. 

Even in relatively large programs, few laboratories will justify the initial expense and calibration effort required for development of the emission spectrographic method. As reported by Scott etal. [3], sample preparation will generally not differ significantly from that required for AAS. Instrumental neutron activation analysis (INAA) is only attractive where a reactor is already available, and multielement analysis by this technique requires the use of high resolution Ge(Li) crystals and multiple irradiations for elements with differing activation product half-lives. The key elements, cadmium, nickel and lead still require analysis by AAS because of limitations of the INAA method [4]. 

A comparative study of the thorium and uranium content in soil samples by gamma spectrometry and neutron activation analysis (NAA) showed a good correlation between the two methods (Anilkumar et al. 2012). The soil samples were dried, powdered, and packed in 250 mL plastic containers, counted for 50,000 with a p-type coaxial HPGe detector that was calibrated. Based on the assumption that was in equilibrium with its daughters, the intensity of the gamma lines at 352 and 609 keV from Pb and respectively, were used to assay the uranium in the... 

Examples of using reference samples for calibration can be found in several chapters of the uses Methods for Geochemical Analysis (Baedecker 1987). Solid reference sample powders are used in cahbrating the dc arc emission, energy-dispersive X-ray and instrumental neutron activation analyses described, while acid-dissolved rock reference samples are used for IGP emission analyses and fused reference samples are used for wavelength-dispersive X-ray analyses. 

Determination of uranium in soil samples can be carried out by nondestructive analysis (NDA) methods that do not require separation of uranium (needed for alpha spectrometry or TIMS) or even digestion of the soil for analysis by ICPMS, ICPAES, or some other spectroscopic methods. These NDA methods can be divided into passive techniques that utilize the natural radioactive mission (gamma and x-ray) of the uranium and progeny radionuclides or active methods where neutrons or electromagnetic radiation are used to excite the uranium and the resultant emissions (gamma, x-rays, or neutrons) are monitored. In many cases, sample preparation is simpler for these nondestructive methods but the requiranent of a neutron source (from a nuclear reactor in many cases) or a radioactive source (x-ray or gamma) and relatively complex calibration and data interpretation procedures make the use of these techniques competitive only in some applications. In addition, the detection limits are usually inferior to the mass spectrometric techniques and the isotopic composition is not readily obtainable. 

Methods of Abundance Measurement. Mass spectrometry (Table 2) is the common form of analysis for lead isotope abundances. Samples suitable for mass spectrometer calibration are in Table 3. Neutron activation ( ° Pb/ ° Pb) and alpha particle activation ( ° Pb/ Pb and ° Pb/ ° Pb) show promise of getting some data on materials having very low lead contents. 

The classical calibration of NAA methods involves comparison of sample activities with those of co-irradiated standards of the same element. Especially at multi-element analysis, the need for a large number of standards has limited the sample throughput capacity. To circumvent this, alternative calibration techniques have been elaborated. The single comparator method makes multi-element determinations possible, by use of a single element standard (neutron flux monitor). The mass of the analyte is calculated by use of an experimentally determined element-specific factor (k-value), valid for the analytical equipment in question (Girardi et al., 1965 Linekin, 1973 Simonits et al., 1975). Later, a more generalized standardization method, based on accurately determined constants for the active compound nuclei (ko-factors), and applicable to various analytical equipments, has been proposed (Moens et al., 1984 De Code et al., 1987). 

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