Nuclear measurements, detection limits

The NAA measurements on the paper samples were made at the Breazeale Nuclear Reactor Facility at the Pennsylvania State University with a TRIGA Mark III reactor at a flux of about 1013 n/cm2-sec. Samples were irradiated from 2 to 20 min and counted for 2000 sec, after a 90 min decay time for Ba and a 60 hr decay for Sb, Analyses were performed instrumentally, without radiochemical separation, using a 35cm3 coaxial Ge-Li detector and a 4096-channel pulse height analyzer. With these procedures, detection limits for Ba and Sb were 0.02ug and 0.001 ug, respectively. These sensitivities are comparable to those obtained by GA s radiochemical separation procedure, and are made possible by the use of the higher neutron output from the more powerful reactor and in combination with the higher resolution solid state detector... 

Elemental mass distribution - The aerosol sampled by the LPI for elemental analysis was impacted on coated mylar films affixed to 25 mm glass discs. The mylar had been coated with Apiezon L vacuum grease to prevent particle bound. The LPI samples were sent to Crocker Nuclear Laboratory for elemental analysis by PIXE using a focused alpha particle beam of 3 to 4 mm diameter. Nanogram sensitivities for most elements were achieved with the focused beam. A detailed description of the PIXE focused beam technique applied to LPI samples can be found in Ouimette (13). Based upon repeated measurements of field samples, the estimated measurement error was about 15-20% or twice the minimum detection limit, whichever was larger. 

Precise and accurate isotope analyses by mass spectrometry have attained growing importance in the last few years due to instrumental improvements with respect to sensitivity, detection limits, precision and accuracy.1 As mentioned before, because the isotope abundances of several elements are not constant and vary as a result of nuclear, biological, chemical, geochemical and physical processes, isotope ratio measurements are required for different research and application fields. Isotope ratio measurements are therefore necessary for elements with two or more isotopes for inves-... 

Helium-3 is a decay product of radioactive tritium (3H, half-life = 12.44 years) that has been produced by nuclear bombs as well as naturally by cosmic rays in the upper atmosphere. Because virtually all 3He atoms escape from the surface ocean to the atmosphere, the 3He/tritium ratio in subsurface seawater samples indicates the time since the water s last exposure to the atmosphere. Both 3He and tritium are measured by gas mass spectrometry. Alternatively, tritium may be measured by gas counting with a detection limit of 0.05 to 0.08 tritium unit, where 1 tritium unit represents a 3H/H ratio of lxl0 18. A degassed water sample is sealed and stored for several months to allow the decay product 3He to accumulate in the container. The amount of 3He is then measured by mass spectrometry, yielding a detection limit of 0.001 to 0.003 tritium unit when 400-gram water samples are used. With this technique, the time since a water mass left the surface can be determined within a range from several months to 30 years. 

Although ICP-MS has been used for analysis of nuclear materials, often the entire instrument must be in an enclosed hot enclosure [350]. Sample preparation equipment, inlets to sample introduction systems, vacuum pump exhaust, and instrument ventilation must be properly isolated. Many of the materials used in the nuclear industry must be of very high purity, so the low detection limits provided by ICP-MS are essential. The fission products and actinide elements have been measured by using isotope dilution ICP-MS [351]. Because isotope ratios are not predictable, isobaric and molecular oxide ion spectral overlaps cannot be corrected mathematically, so chemical separation is required. 

Pajo et al. (2001a) used GD-MS to measure impurities in uranium dioxide fuel and showed that these impurities could be used to identify the original source of confiscated, vagabond nuclear materials. De las Heras et al. (2000) used GD-MS to determine neptunium in Irish Sea sediment samples. The sediment samples were compacted into a disk that was used with a tantalum secondary cathode in the glow discharge. Using a doped marine sediment standard for calibration, detection limits down to the mid pg/g level were determined. 

Sensitive methods for analysis of plutonium in urine are particularly important for estimating occupational plutonium body burdens. Routinely available instrumentation, such as the alpha spectrometer, can readily detect these low concentrations. More sensitive methods are commonly required for urine samples in order to assess chronic exposures to plutonium. These low detection limits were first achieved in the past by nuclear emulsion track counting (see Table 6-1). In this method, the electrodeposited sample is exposed to nuclear track film, subsequent to the isolation of plutonium. The alpha-particle emitting isotopes of plutonium will leave tracks on the film which are counted to quantify the amount of plutonium. Nuclear emulsion track counting has been used in the past to measure plutonium concentrations in the urine of workers at a nuclear reactor plant (Nielsen and Beasley 1980). A type of scintillation counting has been used to measure plutonium-239 and americium-241 in animal tissues (NCRP 1985). 

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