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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.
Past research has shown that anti-coincidence shielded Ge(Li) spectrometers enhanced the signal-to-background ratios for gamma-photopeaks, which are situated on high Compton backgrounds. Ordinarily, an anti- or non-coincidence spectrum (A) and a coincidence spectrum (C) are collected simultaneously with these systems. To be useful in neutron activation analysis (NAA), the fractions of the photopeak counts routed to the two spectra must be constant from sample to sample to variations must be corrected quantitatively. Most Compton suppression counting has been done at low count rate, but in NAA applications, count rates may be much higher. To operate over the wider dynamic range, the effect of count rate on the ratio of the photopeak counts in the two spectra (A/C) was studied. It was found that as the count rate increases, A/C decreases for gammas not coincident with other gammas from the same decay. For gammas coincident with other gammas, A/C increases to a maximum and then decreases. These results suggest that calibration curves are required to correct photopeak areas so quantitative data can be obtained at higher count rates. ?? 1984.
In situ capture gamma-ray analysis in a coal seam using a high resolution gamma-ray spectrometer in a close-fitting borehole has been reported previously. In order to check the accuracy of the method under adverse conditions, similar measurements were made by means of a small-diameter sonde in an oversize borehole in the Pittsburgh seam, Greene County, Pennsylvania. The hole was 5 times the diameter of the sonde, a ratio that substantially increased the contribution of water (hydrogen) to the total spectral count and reduced the size of the sample measured by the detector. The total natural count, the 40K,count, and the intensities of capture gamma rays from Si, Ca, H, and Al were determined as a function of depth above, through, and below the coal seam. From these logs, the depth and width of the coal seam and its partings were determined. Spectra were accumulated in the seam for 1 h periods by using neutron sources of different strengths. From the spectra obtained by means of several 252Cf neutron sources of different sizes, the ultimate elemental analysis and ash content were determined. The results were not as good as those obtained previously in a close-fitting borehole. However, the results did improve with successively larger source-to-detector distances, i.e.,as the count contribution due to hydrogen in the water decreased. It was concluded that in situ borehole analyses should be made in relatively close-fitting boreholes. ?? 1983.
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 Aquia Formation (Paleocene) of Southern Maryland, a marine unit consisting predominantly of quartz sands, but containing 20-40% glauconite, represents one of the many productive, heavily pumped aquifers of the Southeastern Coastal Plain. An unusually high 36Cl activity ( ~ 15 ?? modem water) measured in an outcrop sample is interpreted as a result of the bomb pulse input. About 25 km downdip from the recharge area, a minimum in total chloride concentration occurs. This minimum is thought to correlate with the latest low-stand of sea-level, and thus to provide time information which is in general agreement with ages calculated from hydrodynamic data. However, significant increases in the 36Cl concentrations are observed along the flow path which may be due to ion filtration or to leakage of modem, bomb-contaminated water into the Aquia aquifer. ?? 1987.
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.
In an area in western Tennessee (United States), an industrial firm is injecting acidic (pH = 0.1) iron chloride into permeable zones of carbonate rocks at depths ranging from 1000 to 2200 m below land surface. Overlying the injection zone at a depth of approximately 500 m below land surface is a regional fresh-water aquifer, the Knox aquifer. A study is currently underway to investigate whether the injection wells are hydraulically isolated from the fresh-water aquifer. Drilling of a test well that will reach a total depth of 2700 m has been initiated. The 36Cl content of 15 samples from the Knox aquifer, from monitor wells in the vicinity of the injection site, and from the test well have been analyzed. ?? 1990.
The concentrations of rare earth elements (REEs) in specific mineral grains from the Bayan Obo ore deposit and synthetic high-silica glass samples have been measured by synchrotron X-ray fluorescence (SXRF) analysis using excitation of the REE K lines between 33 and 63 keV. Because SXRF, a nondestructive analytical technique, has much lower minimum detection limits (MDLs) for REEs, it is an important device that extends the in situ analytical capability of electron probe microanalysis (EPMA). The distribution of trace amounts of REEs in common rock-forming minerals, as well as in REE minerals and minerals having minor quantities of REEs, can be analyzed with SXRF. Synchrotron radiation from a bending magnet and a wiggler source at the National Synchrotron Light Source, Brookhaven National Laboratory, was used to excite the REEs. MDLs of 6 ppm (La) to 26 ppm (Lu) for 3600 s in 60-??m-thick standard samples were obtained with a 25-??m diameter wiggler beam. The MDLs for the light REEs were a factor of 10-20 lower than the MDLs obtained with a bending magnet beam. The SXRF REE concentrations in mineral grains greater than 25 ??m compared favorably with measurements using EPMA. Because EPMA offered REE MDLs as low as several hundred ppm, the comparison was limited to the abundant light REEs (La, Ce, Pr, Nd). For trace values of medium and heavy REEs, the SXRF concentrations were in good agreement with measurements using instrumental neutron activation analysis (INAA), a bulk analysis technique. ?? 1993.
A method is presented for assaying radioactive sandstone deposits in situ by using a high-resolution borehole gamma-ray spectrometer. Gamma-ray photopeaks from the same spectrum acquired to analyze a sample are used to characterize gamma-ray attenuation properties, from which a calibration function is determined. Assay results are independent of differences between properties of field samples and those of laboratory or test-hole standards generally used to calibrate a borehole sonde. This assaying technique is also independent of the state of radioactive disequilibrium that usually exists in nature among members of the natural-decay chains. ?? 1985.
We present a new SIngle-scintillator Neutron and Gamma Ray spectrometer (SINGR) instrument for use with both passive and active measurement techniques. Here we discuss the application of SINGR for planetary exploration missions, however, hydrology, nuclear non-proliferation, and resource prospecting are all potential areas where the instrument could be applied. SINGR uses an elpasolite scintillator, Cs 2 YLiCl 6 :Ce (CLYC), that has been shown to have high neutron efficiency even at small volumes, with a gamma-ray energy resolution of approximately 4% full-width-at-half-maximum at 662 keV. Active gamma-ray and neutron (GRNS) measurements were performed with SINGR at the NASA Goddard Space Flight Center (GSFC) Goddard Geophysical and Astronomical Observatory (GGAO) outdoor test site using a pulsed neutron generator (PNG) to interrogate geologically relevant materials (basalt and granite monuments). These experimental results, combined with simulations, demonstrate that SINGR is capable of generating neutron die-away curves that can be used to reconstruct the bulk hydrogen abundance and the depth distribution of hydrogen within the monuments. We compare our experimental results with Monte Carlo N-Particle (MCNP) 6.1 transport simulations to constrain the uncertainties in depth and hydrogen abundance from the neutron die-away data generated by SINGR. For future planetary exploration missions, SINGR provides a single detector system for interrogating the shallow subsurface to characterize the presence and abundance of hydrated phases and to provide bulk elemental analysis.
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.
Chlorine-36 (36Cl) derived from processed nuclear waste that was disposed at the US Department of Energy's Idaho National Engineering and Environmental Laboratory (INEEL) through a deep injection well in 1958, was detected 24-28 yr later in groundwater monitoring wells approximately 26 km downgradient from the source. Groundwater samples covering the period 1966-1995 were selected from the US Geological Survey's archived-sample library at the INEEL and analyzed for 36Cl by accelerator mass spectrometry (AMS). The smaller 36Cl peak concentrations in water from the far-field monitoring wells relative to the input suggest that aquifer dispersivity may be large. However, the sharpness of the 1958 disposal peak of 36Cl is matched by the measured 36Cl concentrations in water from these wells. This implies that a small aquifer dispersivity may be attributed to preferential groundwater flowpaths. Assuming that tracer arrival times at monitoring wells are controlled by preferential flow, a 1-D system-response model was used to estimate dispersivity by comparing the shape of predicted 36Cl-concentration curves to the shape of 36Cl-concentration curves measured in water from these observation wells. The comparisons suggest that a 1-D dispersivity of 5 m provides the best fit to the tracer data. Previous work using a 2-D equivalent porous-media model concluded that longitudinal dispersivity (equivalent to 1-D dispersivity in our model) was 90 m (Ackerman, 1991). A 90 m dispersivity value eliminates the 1958 disposal peak in our model output curves. The implications of the arrival of 36Cl at downgradient monitoring wells are important for three reasons: (1) the arrival times and associated 36Cl concentrations provide quantitative constraints on residence times, velocities, and dispersivities in the aquifer; (2) they help to refine our working hypotheses of groundwater flow in this aquifer and (3) they may suggest a means of estimating the distribution of preferential flowpaths in the aquifer. ?? 2000 Elsevier Science B.V. All rights reserved.
Chlorine-36 (36Cl) concentrations, 36Cl/Cl ratios, and 36Cl fluxes in ice-core samples collected from the Upper Fremont Glacier (UFG) in the Wind River Mountain Range, Wyoming, United States and the Nangpai Gosum Glacier (NGG) in the Himalayan Mountains, Nepal, were determined and compared with published results from the Dye-3 ice-core drilling site on the Greenland Ice Sheet. Cesium-137 (137Cs) concentrations in the NGG also were determined. The background fluxes for 36Cl for each glacial site were similar: (1.6??0.3)??10-2 atoms/cm2 s for the UFG samples, (0.7??0.1)??10-2 atoms/cm2 s for the NGG samples, and (0.4??0.1)??10-2 atoms/cm2 s for the Dye-3 samples. The 36Cl fluxes in ice that was deposited as snow during peak atmospheric nuclear weapon test (1957-1958) were (33??1)??10-2 atoms/cm2 s for the UFG site, (291??3)??10-2 atoms/cm2 s for the NGG site, and (124??5)??10-2 atoms/ cm2 s for the Dye-3 site. A weapon test period 137Cs concentration of 0.79??0.05 Bq/kg in the NGG ice core also was detected in the same section of ice that contained the largest 36Cl concentration. ?? 2000 Elsevier Science B.V. All rights reserved.
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.
In 1991, the U.S. Geological Survey collected a 160-meter (m) ice core from the Upper Fremont Glacier (43??07???N, 109??36???W) in the Wind River Mountain Range of Wyoming in the western United States [1]. In 1994-95, ice from this core was processed at the National Ice Core Laboratory in Denver, Colorado, and analyzed for chlorine-36 (36Cl) by accelerator mass spectrometry at PRIME Laboratory, Purdue University. A tritium bomb peak identified in the work by [1] was used as a marker to estimate the depth of bomb-produced 36Cl. Tritium concentrations ranged from 0 tritium units (TU) for older ice to more than 300 TU at 29 m below the surface of the glacier, a depth that includes ice that was deposited as snow during nuclear-weapons tests through the early 1960's. Maximum 36Cl production during nuclear-weapons tests was in the late 1950's; therefore, the analyses were performed on ice from a depth of 29.8 to 32 m. Calculated flux for 36Cl in ice deposited in the late 1950's ranged from 1.2 ?? 0.1 ?? 10-1 atoms/cm2 s for ice from 29.8 to 30.4 m, to 2.9 ?? 0.1 ?? 10-1 atoms/cm2 s for ice from 31.5 to 32.0 m. Ice samples from a depth of 104.7 to 106.3 m were selected to represent pre-weapons tests 36Cl flux. Calculated flux for 36Cl in this deeper ice was 4.6 ?? 0.8 ?? 10-3 atoms/cm2 s for ice from 104.7 to 105.5 m and 2.0 ?? 0.2 ?? 10-2 atoms/cm2 s for ice from 105.5 to 106.3 m. These flux calculations from the Upper Fremont Glacier analyses are the first for bomb-produced 36Cl in ice from a mid-latitude glacier in North America. It may now be possible to fully quantify the flux of 36Cl from nuclear-weapons tests archived in mid-latitude glacial ice and to gain a better understanding of the distribution of 36Cl and other cosmogenic nuclides.