Technical basis for the reduction of the maximum temperature TGA-MS analysis of oxide samples from the 3013 destructive examination program

Technical Report · Thu Mar 24 00:00:00 EDT 2016

DOI:https://doi.org/10.2172/1244071· OSTI ID:1244071

Scogin, J. H. ^[1]

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1. Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

Thermogravimetric analysis with mass spectroscopy of the evolved gas (TGA-MS) is used to quantify the moisture content of materials in the 3013 destructive examination (3013 DE) surveillance program. Salts frequently present in the 3013 DE materials volatilize in the TGA and condense in the gas lines just outside the TGA furnace. The buildup of condensate can restrict the flow of purge gas and affect both the TGA operations and the mass spectrometer calibration. Removal of the condensed salts requires frequent maintenance and subsequent calibration runs to keep the moisture measurements by mass spectroscopy within acceptable limits, creating delays in processing samples. In this report, the feasibility of determining the total moisture from TGA-MS measurements at a lower temperature is investigated. A temperature of the TGA-MS analysis which reduces the complications caused by the condensation of volatile materials is determined. Analysis shows that an excellent prediction of the presently measured total moisture value can be made using only the data generated up to 700 °C and there is a sound physical basis for this estimate. It is recommended that the maximum temperature of the TGA-MS determination of total moisture for the 3013 DE program be reduced from 1000 °C to 700 °C. It is also suggested that cumulative moisture measurements at 550 °C and 700°C be substituted for the measured value of total moisture in the 3013 DE database. Using these raw values, any of predictions of the total moisture discussed in this report can be made.

• Research Organization: Savannah River Site (SRS), Aiken, SC (United States)
• Sponsoring Organization: USDOE
• DOE Contract Number: AC09-08SR22470
• OSTI ID: 1244071
• Report Number(s): SRNL-STI-2016-00126; TRN: US1601037
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE WASTES FROM NUCLEAR FACILITIES
THERMAL GRAVIMETRIC ANALYSIS
OXIDES
MOISTURE
MASS SPECTROSCOPY
MASS SPECTROMETERS
CALIBRATION
FORECASTING
CONDENSATES
MAINTENANCE
MONITORING
RADIOACTIVE WASTE PROCESSING
REMOVAL
VOLATILITY
TEMPERATURE RANGE 0400-1000 K
GASEOUS WASTES
FEASIBILITY STUDIES