Spectrometry neutron activation

Neutron Activation Spectrometry. Another instrumental technique which has applicability to a wide range of elements is neutron activation analysis. In this method the sample (which could be orange juice without any prior sample treatment) is irradiated with a strong neutron flux. The elements of analytical interest are thus converted to unstable isotopes which decay with characteristic energies and thus measurement of the intensities results in analytical values for the elements of interest. There are some serious drawbacks to this method, however. The matrix can cause severe background effects especially when the sample contains large amounts of an element, like potassium, which is the situation with orange juice. In this event tedious chemical separations must be carried out to achieve adequate selectivity, accuracy... 

TABLE 2. In Vivo Determination of Major and Minor Elements by Neutron Activation Spectrometry... 

Analyses of alloys or ores for hafnium by plasma emission atomic absorption spectroscopy, optical emission spectroscopy (qv), mass spectrometry (qv), x-ray spectroscopy (see X-ray technology), and neutron activation are possible without prior separation of hafnium (19). Alternatively, the combined hafnium and zirconium content can be separated from the sample by fusing the sample with sodium hydroxide, separating silica if present, and precipitating with mandelic acid from a dilute hydrochloric acid solution (20). The precipitate is ignited to oxide which is analy2ed by x-ray or emission spectroscopy to determine the relative proportion of each oxide. 

Numerous methods have been pubUshed for the determination of trace amounts of tellurium (33—42). Instmmental analytical methods (qv) used to determine trace amounts of tellurium include atomic absorption spectrometry, flame, graphite furnace, and hydride generation inductively coupled argon plasma optical emission spectrometry inductively coupled plasma mass spectrometry neutron activation analysis and spectrophotometry (see Mass spectrometry Spectroscopy, optical). Other instmmental methods include polarography, potentiometry, emission spectroscopy, x-ray diffraction, and x-ray fluorescence. 

MetaUic impurities in beryUium metal were formerly determined by d-c arc emission spectrography, foUowing dissolution of the sample in sulfuric acid and calcination to the oxide (16) and this technique is stUl used to determine less common trace elements in nuclear-grade beryUium. However, the common metallic impurities are more conveniently and accurately determined by d-c plasma emission spectrometry, foUowing dissolution of the sample in a hydrochloric—nitric—hydrofluoric acid mixture. Thermal neutron activation analysis has been used to complement d-c plasma and d-c arc emission spectrometry in the analysis of nuclear-grade beryUium. 

The methods of choice for beryUium oxide in beryUium metal are inert gas fusion and fast neutron activation. In the inert gas fusion technique, the sample is fused with nickel metal in a graphite cmcible under a stream of helium or argon. BeryUium oxide is reduced, and the evolved carbon monoxide is measured by infrared absorption spectrometry. BeryUium nitride decomposes under the same fusion conditions and may be determined by measurement of the evolved nitrogen. Oxygen may also be determined by activation with 14 MeV neutrons (20). The only significant interferents in the neutron activation technique are fluorine and boron, which are seldom encountered in beryUium metal samples. 

For the deterrnination of trace amounts of bismuth, atomic absorption spectrometry is probably the most sensitive method. A procedure involving the generation of bismuthine by the use of sodium borohydride followed by flameless atomic absorption spectrometry has been described (6). The sensitivity of this method is given as 10 pg/0.0044M, where M is an absorbance unit the precision is 6.7% for 25 pg of bismuth. The low neutron cross section of bismuth virtually rules out any deterrnination of bismuth based on neutron absorption or neutron activation. 

Thorinm-232 is the only non-radiogenic thorium isotope of the U/Th decay series. Thorinm-232 enters the ocean by continental weathering and is mostly in the particulate form. Early measurements of Th were by alpha-spectrometry and required large volume samples ca. 1000 T). Not only did this make sample collection difficult, but the signal-to-noise ratio was often low and uncertain. With the development of a neutron activation analysis " and amass spectrometry method " the quality of the data greatly improved, and the required volume for mass spectrometry was reduced to less than a liter. Surface ocean waters typically have elevated concentrations of dissolved and particulate 17,3 7,62... 

Another application involves the measurement of copper via the radioisotope Cu (12.6-hour half-life). Since Cu decays by electron capture to Ni ( Cu Ni), a necessary consequence is the emission of X rays from Ni at 7.5 keV. By using X-ray spectrometry following irradiation, sensitive Cu analysis can be accomplished. Because of the short range of the low-energy X rays, near-surface analytical data are obtained without chemical etching. A combination of neutron activation with X-ray spectrometry also can be applied to other elements, such as Zn and Ge. 

Neutron activation also has been combined with accelerator mass spectrometry and has been demonstrated to have part-per-billion sensitivities fer bulk nitrogen analysis in silicon. This combination was also used to obtain depth profile of Cl in silicon semiconductors. ... 

H. Kramer, S. Semel J.E. Abel, Trace Elemental Survey Analysis of Trinitrotoluene , PATR 4767 (1975) (An evaluation of the applicability of spark source mass spectrometry and thermal neutron activation for the detn of origin-related trace elemental impurities in TNT) 10) C. Ribando J. Haber-man, Origin-Identification of Explosives Via Their Composite Impurity Profiles I. The... 

Thermal neutron activation was selected for the radioassay via the soTi(n,7)s 1 Ti reaction. Since the half-life of 51Ti was 5.8 min, nondestructive NAA by gamma-ray spectrometry was used in lieu of chem sepn of Ti... 

Although sophisticated methods may constitute the core methods for certification it is useful to include good, well executed routine methods. In order to further minimize systematic error, a conscious purposeful attempt should be made to get methods and procedures with wide-ranging and different sample preparation steps, including no decomposition as in instrumental neutron activation analysis and particle induced X-ray emission spectrometry. 

Neutron Activation Analysis X-Ray Fluorescence Particle-Induced X-Ray Emission Particle-Induced Nuclear Reaction Analysis Rutherford Backscattering Spectrometry Spark Source Mass Spectrometry Glow Discharge Mass Spectrometry Electron Microprobe Analysis Laser Microprobe Analysis Secondary Ion Mass Analysis Micro-PIXE... 

Chemical Analysis. The chemical composition of ancient objects is important for their authentication. The nature as well as the relative amounts of major, minor, and trace elements in any object are of use for determining the authenticity or otherwise of ceramics, glass, or alloys. A wide range of analytical techniques, depending on the nature of the material studied, have been used for this purpose, including X-rays fluorescence analysis, mass spectrometry, atomic absorption spectroscopy, and neutron activation analy-... 

Many of the published methods for the determination of metals in seawater are concerned with the determination of a single element. Single-element methods are discussed firstly in Sects. 5.2-5.73. However, much of the published work is concerned not only with the determination of a single element but with the determination of groups of elements (Sect. 5.74). This is particularly so in the case of techniques such as graphite furnace atomic absorption spectrometry, Zeeman background-corrected atomic absorption spectrometry, and inductively coupled plasma spectrometry. This also applies to other techniques, such as voltammetry, polarography, neutron activation analysis, X-ray fluroescence spectroscopy, and isotope dilution techniques. 

Various other techniques have been used to determine molybdenum, including adsorption voltammetry [510], electron-paramagnetic resonance spectrometry [512], and neutron activation analysis [513,514]. EPR spectrometry is carried out on the isoamyl alcohol soluble Mo(SCN)s complex and is capable of detecting 0.46 mg/1 molybdenum in seawater. Neutron activation is carried out on the /J-naphlhoin oxime [514] complex and the pyrrolidone dithiocar-bamate and diethyldithiocarbamate complex [513]. The neutron activation analysis method [514] was capable of determining down to 0.32 xg/l of molybdenum in seawater. 

Cerium was included in a list of 14 elements determined by Lee et al. [627] in seawater using neutron activation analysis. The metals were first precon-centraed on a mixture of Chelex 100 and glass powder. The elements were desorbed from the column by 4 M nitric acid, and aqueous solution was irradiated for 3 days and subjected to y-ray spectrometry method with a Ge(Ii) detector coupled to a 4000-channel analyser. Cerium was found to be present to the extent of 16.7 xg/l in water taken from the Kwangyang Bay (South Korea). 

The chemistry of rare earth elements makes them particularly useful in studies of marine geochemistry [637]. But the determination of rare earths in seawater at ultratrace levels has always been a difficult task. Of the various methods applied, instrumental neutron activation analysis and isotope dilution mass spectrometry were the main techniques used for the determination of rare earths in seawater. However, sample preparation is tedious and large amounts of water are required in neutron activation analysis. In addition, the method can only offer relatively low sample throughputs and some rare earths cannot be determined. The main drawbacks of isotopic dilution mass spectrometry are that it is time-consuming and expensive, and monoisotopic elements cannot be determined as well. 

The average concentration and standard deviation of the Pacific Ocean waters ( xg/l) were 2.00 0.09 by neutron activation analysis, and 1.86 0.12 by atomic absorption spectrometry. For the Adriatic water the corresponding values were about 1.7 xg/l. The difference between the values for the same seawater is within the range to be expected from the standard deviations observed. 

Although the neutron activation analysis is inherently more sensitive than the atomic absorption spectrometry, both procedures yield a reliable measurement of vanadium in seawater at the natural levels of concentration. 

Stiller et al. [824] have described the determination of cobalt, copper, and mercury in Dead Sea water by neutron activation analysis followed by X-ray spectrometry and magnetic deflection of /i-ray interference. 

The metals were coprecipitated with lead-ammonium pyrrolidine dithio-carbamate and detected by X-ray spectrometry following neutron activation. Magnetic fields deflect the p rays while the X rays reach the silicon (lithium) detector undeviated. The detectors have low sensitivity to y rays. The concentration of cobalt found by this method was 1.3 xg/l, about one-fifth of that measured previously, while that of copper, 2.0 xg/l, agreed with results obtained by some previous workers. The concentration of mercury was 1.2 xg/l. 

Differentiation of inorganic and organic mercury can be achieved in a number of different ways, many of which depend upon the reduction and vapourisation of the inorganic mercury, followed by reduction [84] or oxidation [85,86] of the organic mercury compounds, and a final measurement by atomic absorption or mass spectrometry. Similar methods of separation of the inorganic and organic components are used in the pretreatment of samples where the final analysis for mercury is to be made by neutron activation analysis [87,88]. 

Asaro, F., Applied Gamma-Ray Spectrometry and Neutron Activation Analysis, Proceedings of the XX. Colloquium Spec-troscopicum Internationale and 7. International Conference on Atomic Spectroscopy Praha 1977 Invited Lectures II, 413-426. 

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