Modern Analytical Techniques in a Nutshell

There are several analytical instruments and techniques that are used to characterize uranium compounds and especially the impurities that accompany them. The modern analytical instrumentation can be divided into two main categories according to 

In this section, we shall first give a simplified description of the principle of operation of the more common analytical techniques that are used to characterize uranium as a major component of a compound or alloy, as a minor component (e.g., in a mineral), as a trace level constituent in an environmental or biological sample and techniques that are used for the determination of other components and impurities in uranium compounds. Frame 1.6 includes quotes from a report that was prepared in 1942 (and declassified in 1947) that compared three analytical techniques for assaying uranium that were considered as state of the art at the time (Mclnnes and Longsworth 1942). 

In a classified report from 1942, which was unclassified and published in 1947, the three main analytical methods that were then used to determine uranium in a sample of hydrated UO3 were compared. One method used prolonged ignition in air in three stages (700°C, 820°C, and 930°C) to form UjO the second involved reduction of the product by hydrogen at 900°C to obtain UO2 and the third included titration with ceric sulfate of uranium sulfate produced by the reaction of UO3 with H2SO4. In their summary, the authors conclude The uranium content of a preparation of hydrated UO3 was determined by three independent procedures... The results of these three methods showed an extreme difference of 0.08%.  

A few variations were also examined, mainly based on titration of overreduced solutions, but these were not as successful as the methods described earlier. The authors state Extensive application of the differential titration method to over-reduced solutions failed to locate the precise end-point of the change. The difficulty is believed to reside with the excessively strong reducing power of the U ion.  

Source Mclnnes, D.A. and Longsworth, L.G., A Comparison of Analytical Methods for the Determination of Uranium, Rockefeller Institute for Medical Research, Oak Ridge, TN, 1942, MDDC-910 (declassified 1947). 

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