Metrology and quality assurance from surveillance of gas compositions over PuO[sub 2] Page: 3 of 11
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Metrology and Quality Assurance for Surveillance of Gas Compositions Over PuO2
criteria because it is believed that the atmosphere will not reach combustible limits. The current
3013 Standard includes a conservative equation for derivation of a bounding pressure increase
based on complete decomposition of water to generate hydrogen. From this equation,
pressurization up to 700 psi can be derived. The equation is conservative and considers only
factors that contribute to pressurization and not those factors that may limit it.
To ensure failures do not occur while the sealed containers are being maintained, a DOE
complex-wide integrated surveillance program is established to define the behavior of these
materials. At Los Alamos National Laboratory (LANL), the Shelf Life Surveillance Project
monitors gases over oxide materials in a limited number of large-scale 3013 inner containers and
in many small-scale containers with samples taken from site-wide representative materials
actually being stored. This information provides invaluable, defensible results for assuring safe
long-term storage of these materials in sealed containers.
The Shelf Life Surveillance Project is a key element of bounding safety scenarios and long-term
surveillance activities for the 3013 containers. Critical to the success of this Surveillance project
are the controls of the Inspection, Measurement, and Test Equipment (IM&TE) and of the data
produced and analyzed from the IM&TE. The Project reviewed all the MD&TE in used for their
affects on quality and data. Only those instruments that contributed directly to the required data
or safety measurements required calibration and were placed on a calibration schedule. Also
since a major "product" of this project is data, quality assurance measures were developed to
specify basic protective measures on the instrumentation and on the quality objectives of the
The LANL shelf-life surveillance project has two parallel studies. Small ten gram samples are
monitored for relatively short time periods, and a limited number of large samples equivalent in
size to the 3013 storage container capacity are monitored for long periods of time. The small
samples will allow a database of many material types prepared according to various site-specific
packaging methods to be compiled. Large-scale studies will give the behavior of a limited
number of samples in the precise geometry and environment in which material will be stored.
Comparison between the two sample geometries will determine the degree of confidence in small
sample experiments and fundamental measurements in predicting the long-term behavior of real
We have designed instrumented storage containers that mimic the inner storage can specified in
the 3013 standard at both large- and small-scale capacities (2.3 liter and 0.0045 liter,
respectively). The containers are designed to maintain the volume to material mass ratio while
allowing the gas composition and pressure to be monitored over time. The large-scale cans are
instrumented with a Raman fiber-optic probe, a gas chromatography (GC) / mass spectrometer
(MS) sampling port, an acoustic resonance chamber, two corrosion monitors, and pressure and
temperature sensors. Data collection for the large-scale containers is automated in order to reduce
worker exposure. The small-scale containers are designed with a microliter gas-sampling
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Worl, L. A. (Laura A.); French, Catherine A. & Kreyer, L. S. (Lawrence S.). Metrology and quality assurance from surveillance of gas compositions over PuO[sub 2], article, January 1, 2002; United States. (digital.library.unt.edu/ark:/67531/metadc932359/m1/3/: accessed January 23, 2019), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.