The nuclear microprobe enables the localization and the quantitative determination of all elements from hydrogen to uranium using atomic and/or nuclear methods: PIXE, PIGE, RBS, ERDA, NRA, STIM, etc. These methods and the apparatus required are shortly described. Three examples show that complementary information is obtained by nuclear microprobe analysis and NAA. The first example is the study of the abnormal behavior of metallic impurities during the purification of metallurgical grade silicon by directional solidification. This behavior is due to the presence of silicon carbide micro-precipitates at the bottom of the ingots. The second example concerns the determination of trace element (Ni, Mn, Rb, Sr) partition coefficients between a solid phase (mineral) and a liquid phase (lava-glass inclusions). These determinations enable the specification and modelling of the processes which govern the magma evolution in volcanological contexts. The third example deals with the study of trace elements in archeological bones. Using PIXE, PIGE, NRA and NAA, it is possible to correlate the concentrations of some elements, such as C, N, F, and Zn in the femoral diaphyse with both the age, the pathology and diagenetic mechanism of the human being at the moment of death.
The degenerations on heat treatment and the thermal stabilities of Na-A molecular sieve zeolites of different crystallinities were studied by thermal analysis. The degenerations of the sieves were computed from the decreases of the zeolitic water content. The thermal stabilities were determined from the commencement of the exothermic peaks. Heating at 600‡ causes considerable degeneration of these sieves. The degeneration and thermal stability depend on the crystallinity of the sieve. Poorly-crystalline sieves are degenerated to a greater extent than well-crystaline ones. The thermal stabilities on poorly-crystalline sieves also decrease during heating at 600‡.
Authors:Kil Lee, Yoon Yoon, Sang Chun, Nak Kim, Keung Park, and Gae Lee
The loss of trace elements during NAA of five liquid reagents, hydrofluoric acid, hydrochloric acid, nitric acid, hydrogen peroxide and deioniyed water, has been investigated using 17 radioactive tracers of46Sc,51Cr,54Mn,59Fe,60Co,645Zn,75Se,85Sr,95Zr,113Sn,124Sb,151Eu,160Yb,177Lu,182Ta,233Pa. Two kinds of container quartz and polyethylene have been used for irradiation and also for preconcentration of the reagents. The containers were cleaned before use by washing-leaching-rinsing procedure. The reagents were preconcentrated by subboiling evaporation under the infrared lamp in clean bench. The loss of trace elements has been revealed to be severer for the reagents of hydrochloric acid and nitric acid in the container of quartz than for the other cases, while that is lowest for hydrogen peroxide.
For simplicity and unification of the comparator methods it is proposed to obtain a calibrating function of changing relative efficiency of registrating -radiation for any geometry of measurement (for any detector) from -spectrum comparator isotopes directly. In determining elements by their short- and medium-lived radionuclides the comparators52V and24Na were used. Biisotope comparator (65Zn,122Eu or182Ta) was used for long-lived radionuclides. The developed universal comparator method significantly simplifies the procedures for determining relative registration efficiencies of analytical lines of interesting radionuclides, thus reducing the labor and time requirements of analysis; this is very important in the case of a large scale NAA.
IAEA standard reference material SOIL-7 has been analyzed by both instrumental NAA and radiochemical NAA using epithermal
neutron activation. These analyses confirm the NAA value of Ag in the intercomparison SOIL-7 which disagrees with some AAS
values. Further geostandards were included and compared with literature data.
A derivative form of NAA is proposed which is based on the use of an endogenous internal standard of already known concentration in the sample. If a comparator with a known ratio of the determinand and endogenous standard are co-irradiated with the sample, the determinand concentration is derived in terms of the endogenous standard concentration and the activity ratios of the two induced nuclides in the sample and comparator. As well as eliminating the sample mass and greatly reducing errors caused by pulse pile-up and geometrical differences, it was shown that in the radiochemical mode, if the endogenous standard is chosen so that the induced activity is radioisotopic with that from the determinand, the radiochemical yield is also eliminated and the risk of non-achievement of isotopic exchange greatly reduced. The method is demonstrated with good results on reference materials for the determination of I, Mn and Ni. The advantages and disadvantages of this approach are discussed. It is suggested that it may be of application in quality control and in extending the range of certified elements in reference materials.
One of the missions of our Institute is the promotion of basic nuclear teaching for students as well as professional teaching
for workers in nuclear industry and research. For nuclear chemistry education, we present here a one day teaching course on
radioactive decay and nuclear reactions, and a two or three days course based on reactor irradiation of uranium oxide, instrumental
and radiochemical analysis of fission products. In the first experiment, the neutron capture is presented as an example of
nuclear reaction; the neutron activation of a silver coin with a Am-Be neutron source, followed by γ-ray spectrometry, is
used to identify three radionuclides of silver and to calculate their half-lives. In the second experiment, our teaching reactor
is used as a neutron source with a flux about 1010 n·cm−2·s−1 at a low thermal power (10 kW). This low flux allows us to irradiate a small uranium sample which is usable for spectrometry
after a short cooling time of about two hours. The first day is reserved for instrumental analysis of the fission products
and a second day for the radiochemical separation of a fission radionuclides. With these experimental results, the students
have to calculate the number of fissions in the irradiated sample. On optional third day for postgraduate students is devoted
to the presentation of NAA and some applications as uranium determination by the fission product spectrometry.
NAA and ICP-MS are both highly sensitive methods for multi-element trace-and ultra-trace element determination. A comparison between analytical figures of merit of both methods is made. Both methods have specific advantages that put them beyond competition for certain applications. It is concluded that ICP-MS can replace NAA for many routine analyses. NAA remains essential as a highly reliable and accurate reference method.
45 elements have been determined by NAA in an IAEA Lake Sediment RM SL-3 Multitechniques were used to fully tap the potential of NAA in terms of the number of the determinable elements and the accuracy of each data.
Authors:A. Grimanis, N. Kalogeropoulos, V. Kilikoglou, and M. Vassilaki-Grimani
Neutron activation analysis (NAA) is a very sensitive and accurate multielement analytical method that is widely applied to the investigation of environmental and archaeological problems. The first part of this paper is a review of pollution studies of toxic trace elements in sediments, seawater and marine organisms of Saronikos Gulf, Greece by NAA. The second part of this paper is a review of provenance studies based on minor and trace element research in ancient ceramics, obsidian, flint, limestone, marble and lead by Instrumental NAA, performed at the NCSR Demokritos.