Thermogravimetry/mass spectrometry is used to identify TG transitions corresponding to loss of residual moisture in freeze-dried biological products with complex TG curves. While TG weight losses were recorded, ion intensities of mass peaksm/e=18 (water) andm/e=44 (carbon dioxide) were monitored continuously for Typhoid Vaccine U.S.P., Meningococcal Polysaccharide Vaccine Groups A and C Combined and Honey Bee Venom Allergenic Extract. MS ion intensities indicated the difference between evolution of residual moisture and moisture associated with product thermal decomposition. Residual moisture values calculated from TG weight losses indicated by mass spectral data agreed with Karl Fischer moisture data.
Authors:C. Hugenschmidt, U. Holzwarth, M. Jansen, S. Kohn, and K. Maier
The crystallization of silica glass has been studied by positron lifetime spectroscopy and accompanying investigations using X-ray diffraction and nuclear magnetic resonance (NMR). To this end isothermal and isochronal heat treatments were performed in the range from 700 °C up to 1600 °C. The lifetime spectra are analyzed by two lifetime components. The decrease of the short lifetime (200 ps) is attributed to the increasing volume fraction of the crystalline phase. The long lifetime (1000 ps) is related with the pick-off annihilation of theo-Ps states in cavities.With starting formation of crystallization nuclei the long lifetime increases which is explained by expanding cavities at the interface between crystalline phase and amorphous matrix.
Authors:L. Wiebe, S. McQuarrie, C. Ediss, W. Maier-Borst, and F. Helus
Liquid scintillation counting of radionuclides emitting beta radiation with Emax>2 MeV has been investigated. Fluor volume effects were similar to those for low energy beta radiation, and pulse height spectra
broadened in a predictable manner with no pulse clipping up to 4.913 MeV. Large changes in sample channels ratio due to color
quenching resulted in progressively smaller losses of counting efficiency as beta energy increased. Counting efficiences were
estimated to be near 100 percent for34Clm,36Cl,32P and38Cl. Cerenkov counting of38Cl by liquid scintillation counter was volume dependent for both counting efficiency and pulse height spectrum. Counting efficiencies
for34Clm,36Cl,32P and38Cl were estimated to be 57.0, 7.5, 42.7 and 66.3%, respectively. Pulse height spectra were shifted to greater pulse heights
as a function of beta Emax, supporting the possibility of energy discrimination for beta emitters by Cerenkov pulse height spectrum analysis. The advantage
of singles Cerenkov counting over coincidence Cerenkov counting was greatest for36Cl and least for38Cl; this advantage was amplified more for samples of36Cl which had been color quenched than for similarly quenched samples of38Cl or32P.
Authors:H. Chen-Mayer, V. Sharov, D. Mildner, R. Downing, R. Paul, R. Lindstrom, C. Zeissler, and Q. Xiao
A neutron lens has been constructed to focus cold neutrons from the exit of a58Ni neutron guide, which delivers a beam to the Prompt-Gamma Activation Analysis (PGAA) station at the NIST Cold Neutron Research Facility. The lens compresses a neutron beam of cross section 50 mm× 45 mm onto a focal spot of diameter 0.53 mm (fwhm) wich an average gain of 80 in neutron current density. PGAA measurements have been performed to demonstrate the enhanced sensitivity and detection limits for various elements and the spatial resolution in one transverse dimension. For the two test particles (a gadolinium glass bead and cadmium metal of sizes less than 0.5 mm), the gain in the -count rate with the lens is a factor of 60, and the detection limit is improved by a factor of 20. The system can be used for two-dimensional mapping of samples on a sub-millimeter scale to complement other analytical techniques such as neutron depth profiling (NDP).