Carrier-Distillation Analysis of Uranium - C&EN Global Enterprise

Nov 5, 2010 - The method was developed at the bureau in 1942 and was used in the Manhattan Project. The bureau has applied the method to control and ...
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Cu ^247 Al 3092 Spectrogram A results from direct arcing of 1 rng. of U.iOs- Uranium spectrum obscures lines of impurities. Spectrogram B, obtained by tfxe carrier-distillation methodfrom 100-mg. samples of U-^Og, shows spectral line? e*/impurities

Carrier-Distillation Analysis of uranium 'ETAILS of a spectrograph^ method of the analysis of uranium and its compounds have recently been announced by B. F. Scribner and H. F. Mullin, chemists of the spectroscopy laboratory a t the National Bureau of Standards. Involving carrierdistillation of the sample, the method per­ mits detection of 33 impurity elements, some in concentrations as low as a few tenths part per million. The method was developed at the bureau i n 1942 and was used in the Manhattan Project. The bureau has applied the method to control and inspection in the production of ura­ nium compounds. Utilization of uranium as a source of atomic energy requiFes material of the Electrode assembly for carrier distilla­ tion analysis of uranium-base materi­ als. When a 10-ampere arc is struck the impurities of the charge are vap­ orized and swept into ~the arc by the **carrier"9 while the vt,ranium oxide remains unvolatilized

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highest purity. I impurities differ in their effects on the nuclear chain reaction. Some elements, sxich as boron and cad­ mium, may interef ere if present in concen­ trations as low a s a few tenths of a part per million, a n d many other elements should not exceeci a few parts per million. Rapid, sensitive, and accurate methods are therefore reqxaired for the determina­ tion of at least 6 0 chemical elements in a variety of uraniixxn-base materials. Prior to 1941, methods for the analysis of ura­ nium to the necessary sensitivity were un­ known. Even -fche established spectro­ graph^ methods of analysis, so useful in general for detecting minute amounts of impurities, were unsuccessful because of interference by tihe highly complex ura­ nium spectrum—s, spectrum in which more than 20,000 l i n e s have been observed. Early in 1941, tz-he bureau, at the request of the Office of Scientific Research and Development, undertook to adapt spec­ trograph! c mettLods to the analysis of uranium. In developing suitable methods it was evident ttLstt the interference of the spectrum of ura^nium, with the spectral lines characteristic of impurities, could be overcome only b y separating the impurities from the u r a n i u m . This was accomplished in the carrier-distillation method by con­ verting the uranixim sample to a refractory compound h a v i n g low volatility (the black oxide of u r a n i u m ΙΓβΟβ) and distilling the impurities from -fchis compound in a direct current electric a^rc. In order to sw^ep- out the minute quan­ tities of i m p u r i t y vapors from the sample without volatilizing the uranium, a small amount of a volatile material, termed a "carrier", is a d d e d to the sample. Gallium oxide, a compoixxid of a rare metal resem­ bling aluminum, was found most useful as a carrier and is a,