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Organisationseinheit der BAM
In the second part of this two-part series on the state-of-the-art comparability of corrected emission spectra, we have extended this assessment to the broader community of fluorescence spectroscopists by involving 12 field laboratories that were randomly selected on the basis of their fluorescence measuring equipment. These laboratories performed a reference material (RM)-based fluorometer calibration with commercially available spectral fluorescence standards following a standard operating procedure that involved routine measurement conditions and the data evaluation software LINKCORR developed and provided by the Federal Institute for Materials Research and Testing (BAM). This instrument-specific emission correction curve was subsequently used for the determination of the corrected emission spectra of three test dyes, X, QS, and Y, revealing an average accuracy of 6.8% for the corrected emission spectra. This compares well with the relative standard uncertainties of 4.2% for physical standard-based spectral corrections demonstrated in the first part of this study (previous paper in this issue) involving an international group of four expert laboratories. The excellent comparability of the measurements of the field laboratories also demonstrates the effectiveness of RM-based correction procedures.
The development of fluorescence applications in the life and material sciences has proceeded largely without sufficient concern for the measurement uncertainties related to the characterization of fluorescence instruments. In this first part of a two-part series on the state-of-the-art comparability of corrected emission spectra, four National Metrology Institutes active in high-precision steady-state fluorometry performed a first comparison of fluorescence measurement capabilities by evaluating physical transfer standard (PTS)-based and reference material (RM)-based calibration methods. To identify achievable comparability and sources of error in instrument calibration, the emission spectra of three test dyes in the wavelength region from 300 to 770 nm were corrected and compared using both calibration methods. The results, obtained for typical spectrofluorometric (0°/90° transmitting) and colorimetric (45°/0° front-face) measurement geometries, demonstrated a comparability of corrected emission spectra within a relative standard uncertainty of 4.2% for PTS- and 2.4% for RM-based spectral correction when measurements and calibrations were performed under identical conditions. Moreover, the emission spectra of RMs F001 to F005, certified by BAM, Federal Institute for Materials Research and Testing, were confirmed. These RMs were subsequently used for the assessment of the comparability of RM-based corrected emission spectra of field laboratories using common commercial spectrofluorometers and routine measurement conditions in part 2 of this series (subsequent paper in this issue).
Specific attention should be paid on safety demonstrations transmitted by applicants in the case of approval request for the package designs containing enriched UF6. Concerning the shipment of enriched UF6, the package designs consist in general of a filled 30B cylinder surrounded by an overpack.
The description of the content, considering the UF6 origin, i.e. natural or reprocessed, shall be clearly justified especially when the UF6 isotopic composition exceeds the limits specified in ASTM standards.
Concerning the containment of the UF6, the applicant shall demonstrate in all conditions of Transport the leak-tightness of the valve and plug of the cylinders filled with enriched UF6. In this regard, when justifications are based on numerical calculations, the absence of contact between These components of the cylinder and the internal surfaces of the overpack after the regulatory drop tests shall be shown. In particular, absence of contact between the valve and any other component of the packaging shall be confirmed to respect the current IAEA regulations [3]. If complementary calculations show a contact between the plug and the internal surfaces of the overpack, additional tests are required to confirm that the strength resulting from this contact will not affect the plug leak-tightness. It can be noticed that the future revision of the IAEA regulations will include additional provision in case of contact of the plug with any other component of the packaging. In addition, the applicant shall demonstrate that the melting temperature of the valve, including the tinned joint, will not be exceeded during the regulatory fire test.
Furthermore, the representativeness of the ballast used to simulate the behaviour of the UF6 loaded within the cylinder shall be justified if drop tests are performed.
Finally, specific provisions relative to the use of plugs and the maintenance of cylinders should be included in the safety analysis reports.
The safety demonstrations realized by applicants in the case of approval request for the package designs containing enriched UF6 have to take into account some specific technical issues. Concerning the shipment of enriched UF6, the package designs consist in general of a filled 30B cylinder surrounded by an overpack.
The description of the content, considering the UF6 origin, i.e. natural or reprocessed, shall be clearly justified especially when the UF6 isotopic composition exceeds the limits specified in ASTM standards.
Concerning the containment of the UF6, the applicant shall demonstrate in all conditions of transport the leak-tightness of the valve and plug of the cylinders filled with enriched UF6. In this regard, when mechanical justifications are based on numerical calculations, the absence of contact between these components of the cylinder and the internal surfaces of the overpack after the regulatory drop tests shall be shown to respect the IAEA regulations.
Furthermore, the representativeness of the ballast used to simulate the behaviour of the UF6 loaded within the cylinder shall be justified if drop tests are performed. The representativeness of the ballast should also be justified for numerical calculations.
In addition, the applicant shall demonstrate that the melting temperature of the valve and the plug, including the tinned joint, will not be exceeded during the regulatory fire test.
Finally, specific provisions relative to the use of plugs and the maintenance of cylinders should be included in the safety analysis report.