Neutron emission

Corpuscular emission (neutrons, protons, electrons, positrons) + + ... 

TJecent interest in the trace element content of coal has increased the need for rapid and accurate analytical methods for their determination. Because x-ray fluorescence analysis has demonstrated its usefulness in determining major, minor, and trace elements in numerous other types of materials, it was felt that this method could be extended to trace element determinations in whole coal. In the past, such analyses were seriously hampered by the lack of standard samples. However, research being conducted in our laboratories under the sponsorship of the U. S. Environmental Protection Agency produced a large number of coal samples for which trace elements had been determined by two or more independent analytical procedures, for example, optical emission, neutron activation, atomic absorption, and wet chemical methods. These coals were used as standards to develop an x-ray fluorescence method that would determine many trace and minor elements in pressed whole coal samples. 

Type Reaction Half-life Neutron emission (neutrons/curie/sec)... 

The methods used can be conveniently arranged into a number of categories (a) fractionation by precipitation (b) fractionation by distillation (c) separation by chromatographic techniques (d) chemical analysis by spectrophotometric techniques (infrared, ultraviolet, nuclear magnetic resource. X-ray fluorescence, emission, neutron activation), titrimetric and gravimetric techniques, and elemental analysis and (e) molecular weight analysis by mass spectrometry, vapor pressure osmometry, and size exclusion chromatography. 

For trace quantities of less than 100 ppm, the most successful method — and the most costly— is neutron activation. The sample is subjected to neutron bombardment in an accelerator where oxygen 16 is converted to unstable nitrogen 16 having a half-life of seven seconds. This is accompanied by emission of (J and 7 rays which are detected and measured. Oxygen concentrations as low as 10 ppm can be detected. At such levels, the problem is to find an acceptable blank sample. 

The discoveries at Berkeley were made by bombarding a target of 249Cf with 12C nuclei of 71 MeV, and 13C nuclei of 69 MeV. The combination of 12C with 249Cf followed by instant emission of four neutrons produced Element 257-104. This isotope has a half-life of 4 to 5 s. 

The same reaction, except with the emission of three neutrons, was thought to have produced 258-104 with a half-life of about 1/100 s. 

Element 259-104 is formed by the merging of a 13C nuclei with 249Cf, followed by emission of three neutrons. This isotope has a half-life of 3 to 4 s, and decays by emitting an alpha particle into 255No, which has a half-life of 185 s. 

When hydrogen is burned up in the nuclear furnace of a star, helium burning takes over, forming carbon, which in turn leads to oxygen, etc. Subsequent emission processes releasing a-particles, equilibrium processes, neutron absorption, proton capture, etc. lead to heavier elements. 

Converting a proton to a neutron results in the emission of a positron, i[3. 

Neutron Activation Analysis Few samples of interest are naturally radioactive. For many elements, however, radioactivity may be induced by irradiating the sample with neutrons in a process called neutron activation analysis (NAA). The radioactive element formed by neutron activation decays to a stable isotope by emitting gamma rays and, if necessary, other nuclear particles. The rate of gamma-ray emission is proportional to the analyte s initial concentration in the sample. For example, when a sample containing nonradioactive 13AI is placed in a nuclear reactor and irradiated with neutrons, the following nuclear reaction results. 

The concentration of Mn in steel can be determined by a neutron activation analysis using the method of external standards. A 1.000-g sample of an unknown steel sample and a 0.950-g sample of a standard steel known to contain 0.463% w/w Mn, are irradiated with neutrons in a nuclear reactor for 10 h. After a 40-min cooling period, the activities for gamma-ray emission were found to be 2542 cpm (counts per minute) for the unknown and 1984 cpm for the standard. What is the %w/w Mn in the unknown steel sample ... 

Determination of gold concentrations to ca 1 ppm in solution via atomic absorption spectrophotometry (62) has become an increasingly popular technique because it is available in most modem analytical laboratories and because it obviates extensive sample preparation. A more sensitive method for gold analysis is neutron activation, which permits accurate determination to levels < 1 ppb (63). The sensitivity arises from the high neutron-capture cross section (9.9 x 10 = 99 barns) of the only natural isotope, Au. The resulting isotope, Au, decays by P and y emission with a half-life of 2.7 d. 

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. 

Ca(I) sites have been shown to be responsible for most of the observed luminescence, whereas emission from the Mn " ions on the Ca(Il) sites occur only for higher Mn concentrations. Neutron diffraction studies have also confirmed these results (10). 

There are four modes of radioactive decay that are common and that are exhibited by the decay of naturally occurring radionucHdes. These four are a-decay, j3 -decay, electron capture and j3 -decay, and isomeric or y-decay. In the first three of these, the atom is changed from one chemical element to another in the fourth, the atom is unchanged. In addition, there are three modes of decay that occur almost exclusively in synthetic radionucHdes. These are spontaneous fission, delayed-proton emission, and delayed-neutron emission. Lasdy, there are two exotic, and very long-Hved, decay modes. These are cluster emission and double P-decay. In all of these processes, the energy, spin and parity, nucleon number, and lepton number are conserved. Methods of measuring the associated radiations are discussed in Reference 2 specific methods for y-rays are discussed in Reference 1. 

Although protons and neutrons are not emitted from the ground states of these isotopes, there are many cases where particles are emitted from excited states. For example, Cs decays by electron capture and -emission to excited levels ia and ia 7% of these cases protons are emitted from... 

Cluster emission is an exotic decay that has some commonalities with a-decay. In a-decay, two protons and two neutrons that are moving in separate orbits within the nucleus come together and leak out of the nucleus as a single particle. Cluster emission occurs when other groups of nucleons form a single particle and leak out. Several of the observed decays are shown in Table 10. The emitted clusters include C, Ne, Mg, and Si. The... 

The isotopes produced by reactors are not common as biological markers. The absorption of neutrons generally results in radioisotopes (qv) that He below the line of stabiUty on the chart of the nucHdes. These tend to decay by j3 -emission, an undesirable mode for a diagnostic. 

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. 

In NAA the sample is made radioactive by subjecting it to a high dose (days) of thermal neutrons in a reactor. The process is effective for about two-thirds of the elements in the periodic table. The sample is then removed in a lead-shielded container. The radioisotopes formed decay by B emission, y-ray emission, or X-ray emission. The y-ray or X-ray energies are measured by EDS (see Chapter 3) in spe-... 

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. 

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