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A high pressure-temperature press is used to make target material for accelerator mass spectrometry. Graphite was produced from typical **1**4C samples including oxalic acid and carbonates. Beam strength of **1**2C was generally adequate, but random radioactive contamination by **1**4C made age measurements impractical.
A sonde has been built for high-resolution measurement of natural or neutron-induced gamma rays in boreholes. The sonde is 7.3 cm in diameter and about 2.2 m in length and weighs about 16 kg. The lithium-compensated germanium semiconductor detector is stabilized at −185 to −188°C for as much as ten hours by a cryostatic reservoir containing melting propane. During periods when the sonde is not in use the propane is kept frozen by a gravity-fed trickle of liquid nitrogen from a reservoir temporarily attached to the cryostat section. A 252 Cf source, shielded from the detector, may be placed in the bottom section of the sonde for anlysis by measurement of neutron-activation or neutron-capture gamma rays. Stability of the cryostat with changing hydrostatic pressure, absence of vibration, lack of need for power to the cryostat during operation, and freedom of orientation make the method desirable for borehole, undersea, space, and some laboratory applications.
The linear combination technique, when applied to a gamma-ray spectrum, gives a single number indicative of the extent to which the spectral lines of a sought element are present in a complex spectrum. Spectra are taken of the sought element and of various other substances whose spectra interfere with that of the sought element. A weighting function is then computed for application to spectra of unknown materials. The technique was used to determine calcium by radiative-neutron-capture gamma-ray analysis in the presence of interfering elements, notably titanium, and the results were compared with those for two popular methods of peak area integration. Although linearity of response was similar for the methods, the linear combination technique was much better at rejecting interferences. For analyses involving mixtures of unknown composition the technique consequently offers improved sensitivity.
Both an accelerator and a 252 Cf neutron source have been used to induce characteristic gamma radiation from extended soil samples. To demonstrate the method, measurements of the neutron-induced radiative capture and activation gamma rays have been made with both Ge(Li) and NaI(Tl) detectors, Because of the possible application to space flight geochemical analysis, it is believed that NaI(Tl) detectors must be used. Analytical procedures have been developed to obtain both qualitative and semiquantitative results from an interpretation of the measured NaI(Tl) pulse-height spectrum. Experiment results and the analytic procedure are presented.
In situ -produced 10 Be in quartz is widely used to constrain exposure ages and denudation rates, traditionally measured in sand-sized grains. Here we report a new method for isolating fine-grained quartz from shale and demonstrate its reliability for grain sizes down to single microns. Sequential dissolution tests and analyses of grain size separates show that meteoric 10 Be is eliminated and that recoil losses during cosmogenic nuclide production are balanced by implantation from other mineral grains. High-temperature combustion leads to diffusion of meteoric 10 Be into fine-grained quartz and must be used with caution.
90Sr (T1/2 = 28.5 years) is a long-lived radionuclide produced in nuclear fission. Fast radiochemical detection of 90Sr in environmental samples is not feasible using current analytical methods. Accelerator Mass Spectrometry (AMS) measurements of 90Sr were made with the Rehovot 14UD Pelletron accelerator at a terminal voltage of 11 or 12 MV using our standard detection system. Injection of hydride ions (SrH3-) was chosen owing to high beam intensity and low Coulomb explosion effects. 90Sr ions were identified and discriminated from isobaric 90Zr by measuring time of flight, total energy and three independent energy-loss signals in an ionization chamber. A reference sample and a ground-water sample were successfully measured. The detection limit determined for a laboratory blank by the residual counts in the 90Sr region is 90Sr/Sr = 3 ?? 10-13, corresponding in practice to (2-4) ?? 10790Sr atoms or about 0.5-1 pCi/L in environmental water samples.
From experimental studies of gamma rays from fast and thermal neutron reactions in hydrogeneous and non-hydrogeneous, semi-infinite samples and from Monte Carlo calculations on soil of a composition which might typically be encountered on planetary surfaces, it is found that gamma rays from fast or inelastic scattering reactions would dominate the observed spectra. With the exception of gamma rays formed by inelastically scattered neutrons on oxygen, useful spectra would be limited to energies below 3 MeV. Other experiments were performed which show that if a gamma-ray detector were placed within 6 m of an isotopic neutron source in a spacecraft, it would be rendered useless for gamma-ray spectrometry below 3 MeV because of internal activation produced by neutron exposure during space travel. Adequate shielding is not practicable because of the size and weight constraints for planetary missions. Thus, it is required that the source be turned off or removed to a safe distance during non-measurement periods. In view of these results an accelerator or an off-on isotopic source would be desirable for practical gamma-ray spectral analysis on planetary surfaces containing but minor amounts of hydrogen.
A feasibility study has been made to operate by remote control an unshielded portable positive-ion accelerator type neutron source to induce activities in the ground or rock by “in situ” neutron irradiation. Selective activation techniques make it possible to detect some thirty or more elements by irradiating the ground for periods of a few minutes with either 3-MeV or 14-MeV neutrons. The depth of penetration of neutrons, the effect of water content of the soil on neutron moderation, gamma ray attenuation in the soil and other problems are considered. The analysis shows that, when exploring for most elements of economic interest, the reaction 2 H(d,n) 3 He yielding ∼ 3-MeV neutrons is most practical to produce a relatively uniform flux of neutrons of less than 1 keV to a depth of 19″–20″. Irradiation with high energy neutrons (∼ 14 MeV) can also be used and may be better suited for certain problems. However, due to higher background and lower sensitivity for the heavy minerals, it is not a recommended neutron source for general exploration use. Preliminary experiments have been made which indicate that neutron activation in situ is feasible for a mineral exploration or qualititative soil analysis.
A table of the analytical sensitivities of the principal lines in the thermal-neutron-capture gamma ray spectrum has been compiled for most of the elements. In addition a second table of the full-energy, single-escape, and double-escape peaks has been compiled according to energy for all significant lines above 3 MeV. Lines that contrast well with adjacent lines are noted as prominent. The tables are useful for spectral interpretation and calibration.
A table of the analytical sensitivities of the principal lines in the thermal neutron capture gamma-ray spectrum from 0 to 3 MeV has been compiled for most of the elements. A tabulation of the full-energy, single-escape, and double-escape peaks has also been made according to energy. The tables are useful for spectral interpretation and calibration.
High resolution intrinsic and lithium-drifted germanium gamma-ray detectors operate at about 77–90 K. A cryostat for borehole and marine applications has been designed that makes use of prefrozen propane canisters. Uses of such canisters simplifies cryostat construction, and the rapid exchange of canisters greatly reduces the time required to restore the detector to full holding-time capability and enhances the safety of a field operation where high-intensity 252 Cf or other isotopic sources are used. A holding time of 6 h at 86 K was achieved in the laboratory in a simulated borehole probe in which a canister 3.7 cm diameter by 57 cm long was used. Longer holding times can be achieved by larger volume canisters in marine probes.
A borehole sonde (~1.7 m long; 7.3 cm diameter) using a 200 mm 2 planar intrinsic germanium detector, mounted in a cryostat cooled by removable canisters of frozen propane, has been constructed and tested. The sonde is especially useful in measuring X- and low-energy gamma-ray spectra (40–400 keV). Laboratory tests in an artificial borehole facility indicate its potential for in-situ uranium analyses in boreholes irrespective of the state of equilibrium in the uranium series. Both natural gamma-ray and neutron-activation gamma-ray spectra have been measured with the sonde. Although the neutron-activation technique yields greater sensitivity, improvements being made in the resolution and efficiency of intrinsic germanium detectors suggest that it will soon be possible to use a similar sonde in the passive mode for measurement of uranium in a borehole down to about 0.1% with acceptable accuracy. Using a similar detector and neutron activation, the sonde can be used to measure uranium down to 0.01%.
Trace elements in coal can occur as components of either the organic constituents (macerals) or the inorganic constituents (minerals). Studies of the concentrations and distribution of the trace elements are vital to understanding the geochemical millieu in which the coal was formed and in evaluating the attempts to recover rare but technologically valuable metals. In addition, information on the trace element concentrations is important in predicting the environmental impact of burning particular coals, as many countries move toward greater utilization of coal reserves for energy production. Traditionally, the optical and the electron microscopes and more recently the electron microprobe have been used in studying the components of coal. The proton-induced X-ray emission (PIXE) microprobe offers a new complementary approach with an order of magnitude or more better minimum detection limit. We present the first measurements with a PIXE microprobe of the trace element concentrations of bituminous coal samples. Elemental analyses of the coal macerals-vitrinite, exinite, and inertinite-are discussed for three coal samples from the Eastern U.S.A., three samples from the Western U.S.A., and one sample from the Peoples Republic of China. ?? 1981.
A neutron generator pulsed at 100 s-1 was suspended in an artificial borehole containing a 7.7 metric ton mixture of sand, aragonite, magnetite, sulfur, and salt. Two Ge(HP) gamma-ray detectors were used: one in a borehole sonde, and one at the outside wall of the sample tank opposite the neutron generator target. Gamma-ray spectra were collected by the outside detector during each of 10 discrete time windows during the 10 ms period following the onset of gamma-ray build-up after each neutron burst. The sample was measured first when dry and then when saturated with water. In the dry sample, gamma rays due to inelastic neutron scattering, neutron capture, and decay were counted during the first (150 ??s) time window. Subsequently only capture and decay gamma rays were observed. In the wet sample, only neutron capture and decay gamma rays were observed. Neutron capture gamma rays dominated the spectrum during the period from 150 to 400 ??s after the neutron burst in both samples, but decreased with time much more rapidly in the wet sample. A signal-to-noise-ratio (S/N) analysis indicates that optimum conditions for neutron capture analysis occurred in the 350-800 ??s window. A poor S/N in the first 100-150 ??s is due to a large background continuum during the first time interval. Time gating can be used to enhance gamma-ray spectra, depending on the nuclides in the target material and the reactions needed to produce them, and should improve the sensitivity of in situ well logging. ?? 1984.
The use of 236U and 229Th in alpha spectrometric measurements has some advantages over the use of other tracers and measurement techniques in isotope dilution analyses of most geological samples. The advantages are: (1) these isotopes do not occur in terrestrial rocks, (2) they have negligible decay losses because of their long half lives, (3) they cause minimal recoil contamination to surface-barrier detectors, (4) they allow for simultaneous determination of the concentration and isotopic composition of uranium and thorium in a variety of sample types, and (5) they allow for simple and constant corrections for spectral inferences, 0.5% of the 238U activity is subtracted for the contribution of 235U in the 236U peak and 1% of the 229Th activity is subtracted from the 230Th activity. Disadvantages in using 236U and 229Th are: (1) individual separates of uranium and thorium must be prepared as very thin sources for alpha spectrometry, (2) good resolution in the spectrometer system is required for thorium isotopic measurements where measurement times may extend to 300 h, and (3) separate calibrations of the 236U and 229Th spike solution with both uranium and thorium standards are required. The use of these tracers in applications of uranium-series disequilibrium studies has simplified the measurements required for the determination of the isotopic composition of uranium and thorium because of the minimal corrections needed for alpha spectral interferences. ?? 1984.
The variations with depth of the elemental concentrations in vitrinites in a series of vitrites have been determined using radiation from the Cornell high energy synchrotron source. All of the vitrites were selected from a single drill core sample of coal from the Emery coalfield, Utah. The results are compared with similar determinations using the Heidelberg proton microprobe. The advantages and disadvantages of the two techniques are discussed. Results are reported for S, Ca, Ti, Fe, Zn, Br, and Sr. For example, it is found that Fe increases from top to bottom of the coal bed in contrast to S, which decreases from top to bottom of the bed. Other features of the two data sets are also described. ?? 1984.
The occurrence of the so-called invisible gold in two unoxidized Carlin-type gold samples from Nevada has been determined using synchrotron X-ray fluorescence (SXRF) analysis at the National Synchrotron Light Source, Brookhaven National Laboratory. A bedded sample from the East ore zone of the Carlin deposit and a breccia sample from Horse Canyon were analyzed. Preliminary results show that gold is found only in the Horse Canyon breccia sample. Experimental details including other X-ray line and diffraction peak interferences, standards used, and minimum detection limits (MDLs) are discussed. Gold, with a MDL range of 0.8 to 3 ppm, was not detected in euhedral pyrite crystals except in the interior porous portion of one grain. Gold was detected in some parts of the matrix. The phase which contains gold has not yet been identified. The highest content of gold so far analyzed is about 40 ppm. There are interesting implications of these new findings. ?? 1987.
Synchrotron radiation sources offer important features for the analysis of a material. Among these features is the ability to determine both the elemental composition of the material and the chemical state of its elements. For microscopic analysis synchrotron X-ray fluorescence (SXRF) microprobes now offer spatial resolutions of 10 ??m with minimum detection limits in the 1-10 ppm range depending on the nature of the sample and the synchrotron source used. This paper describes the properties of synchrotron radiation and their importance for elemental analysis, existing synchrotron facilities and those under construction that are optimum for SXRF microanalysis, and a number of applications including the high energy excitation of the K lines of heavy elements, microtomography, and XANES and EXAFS spectroscopies. ?? 1990.