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Some Reminiscences of Mass Spectrometry and the Manhattan Project

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Some Reminiscences of Mass Spectrometry and the Manhattan Project Reflections on Nuclear Fission at Its Half-Century Some Reminiscences of Mass Spectrometry and the Manhattan Project Alfred O. Nier School of Physics and Astronomy, University of Minnesota, Minneapolis, MN 55455 Prior to World War II there were only a few mass spectro- mg two tons and a 5 kW generator with a stabilized output meters in the entire world, and these were built by scientists voltage to power it. Whereas, in my previous apparatus (1) who used them as tools in their own research, studying the the mass spectrometer “tube” was mounted inside of a sole- dissociation and ionization of molecules by electron impact noid, limiting both the magnetic field and radius of curva- or determining the relative abundances of isotopes. The ture of the ions, and hence limiting the obtainable mass need of the petroleum industry to find better means for resolution, in the new instrument the tube was mounted analyzing complex hydrocarbon mixtures and the uranium between the poles of the magnet. The combination of the isotope separation and atomic bomb production program larger possible radius of curvature and stronger magnetic (known as the Manhattan Project) stimulated the design field gave appreciably higher resolution as well as general and construction of new improved mass spectrometers. Fol- performance. Figure 1 is a schematic drawing of the mass lowing the war such instrumentation became widely avail- spectrometer tube employed (2). able commercially and applicable to a wide range of prob- Cambridge, Massachusetts, was an exciting place to be in lems such as gas analyses, use of isotopic tracers in chemical, the 1930’s for one interested in geological age determina- biological or medical science, and determination of isotopic tions. Alfred Lane, a retired professor of geology from Tufts abundance in samples of geological or cosmological interest. College, was chairman of the National Research Council’s This is an account of some of the author’s experiences during Committee on the Measurement of Geological Time, and the transformation of this rather rare form of instrumenta- very active in promoting the work of the committee. At MIT tion from an exotic tool of specialists to a device having there was Robley Evans and his group, working on the radio- universal application. activity of minerals, and at Harvard, in chemistry, there was When I completed my graduate studies in physics at Min- Gregory Baxter, the atomic weight authority and successor nesota in 1936,1 had the good fortune to receive a National to T. W. Richards. Baxter and his students had made atomic Research Council Fellowship, and elected to spend my two weight measurements on numerous lead samples extracted years at Harvard working with Kenneth Bainbridge. For my from uranium and thorium minerals and had a marvelous thesis I had measured the relative abundances of the iso- collection of these samples and ones of common lead as well topes of a few elements—argon, potassium, zinc, rubidium, as material studied earlier by Richards. and cadmium. Bainbridge, who was an authority on the The of Uranium precise measurement of isotopic masses, suggested I might Isotopic Composition wish to extend my abundance measurements to the heavy At the time, the isotopic abundance ratio, 238U/235U, was elements, particularly lead and uranium, of interest in the not known even within a factor of two. 235U had only been determination of the ages of minerals by radioactive decay identified mass spectroscopically by Dempster (3) a few methods. He helped me design a mass spectrometer that years before, and its abundance roughly estimated from the could readily measure isotopic abundance ratios throughout blackening of a line on a photographic plate. An accurate the entire atomic table. It required an electromagnet weigh- knowledge of the isotopic abundance ratio was of great im- portance for radioactive dating. I felt that with a sample of a volatile uranium compound such as UFg a successful deter- Downloaded via CALIFORNIA INST OF TECHNOLOGY on January 18, 2019 at 18:13:40 (UTC). See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles. mination might be made, and Lane, armed with a $500 grant he had obtained on my behalf from the Geological Society of America, looked for a prospective provider. He was unsuc- cessful and the money reverted. Fortunately, Baxter came to the rescue, providing samples of UCI4 and UBr4, which are volatile at elevated temperatures. The well-known ratio, 238U/a35U = 139 (now given more accurately as 137.8), result- ed from the measurements. Figure 2 shows a mass spectrum obtained in this early work (4). The measurements were sufficiently good to show even the rare isotope, 234U, in radioactive equilibrium with 23aU, and having an abundance of only 1 part in 17,000 in uranium. The Sector Magnet Mass Spectrometer In the fall of 1938, when my NRC fellowship expired, I was offered and accepted a faculty position back at Minnesota. Figure 1. Schematic views of 180° magnetic deflection mass spectrometer John who had been me started tube, tons are produced by electrons emitted from a heated filament F and Tate, my adviser, helped get in research me with funds so I could passing between plates D and B before being collected on plate E (edge view my again by providing of lube). Mass spectra are obtained by sweeping the ion accelerating potential have a 2-ton magnet similar to the one 1 had at Harvard, and impressed between plates B and C. The analyzed ion currents are measured- Bainbridge allowed me to keep the mass spectrometer tubes with an electrometer tube amplifier connected to collector plate P. I had built at Harvard. As a result, I was back in operation in Volume 66 Number 5 May 1989 385 . about 6 months and continued some of the lead-age work I after the discovery of nuclear fission, which was a lively topic had started at Harvard. of discussion at the meeting. I already knew John Dunning Now, however, there were other interests as well. Clusius at Columbia University, and he introduced me to Fermi. At and Dickel in Germany (5) had demonstrated that with a the time it had not been experimentally demonstrated that thermal diffusion column one could separate isotopes. This 235U was responsible for the slow neutron fission of uranium, seemed an interesting field to enter, especially since we had a as had been predicted by Bohr and Wheeler (8), so a direct mass spectrometer that could monitor the performance of measurement was of some interest. Because of the high cross isotope separation methods. We built a column that ulti- section for the slow neutron fission it appeared that by mately produced methane enriched by a factor of over 10 in running my 180° mass spectrometer with more intense ion 13C (6). The material was of great interest to biologists, who beams it should be possible to isolate enough 235U to make could use it for tracer studies. As a result I gained many new possible a test. friends, and my students and I, in addition to performing our Following the meeting I returned to Minneapolis, but be- own research, found ourselves producing enriched 13C and tween lecturing 8 hours per week, perfecting the sector mag- running analyses for our colleagues in physiology and bot- net mass spectrometer, trying to separate 13C by thermal any. diffusion, and continuing our study of uranium lead sam- At the time, we had one of the few mass spectrometers in ples, I was not looking for things to do, so the separation of existence capable of making precise isotope analyses. It was 235U was not high on my priority list. Dunning kept after me, clear we needed more instruments—preferably ones which as did Fermi in a letter that is one of my prized possessions, a did not use 2-ton magnets requiring 5 kW voltage-stabilized copy of which is shown as Figure 4. generators for providing the magnet current. This led to the To accomplish the separation I proposed using UF0, a development of the sector magnet mass spectrometer (7), in relatively volatile compound and now available, as a source which a 60° sector magnet took the place of the much larger of uranium that could be ionized. The Columbia group pro- one needed to give a 180° deflection. The upshot was that a vided me with some, which I tried over the Christmas holi- magnet weighing a few hundred pounds, and powered by days and into early February 1940. Unfortunately, UF0, be- several automobile storage batteries, took the place of the 2- ing a highly volatile compound, coated most of the surfaces ton magnet with its 5-kW generator. Figure 3 is a photo- of the mass spectrometer tube, including the ion collector graph of the original instrument, completed in 1939, which targets, so the tests were unsuccessful. Finally, in February I was destined to be the prototype for all subsequent magnetic built an entirely new mass spectrometer tube and went back deflection instruments, including the hundreds used on the to using UBr4, which was volatile only when heated. Fortu- Manhattan Project for a variety of purposes. nately, I had some left over from my Harvard days. An oven was built into the ion source, as had been done in a previous of 235U Mass Separation by Spectrometry isotopic study of low volatility elements (9), and the vapor I attended the American Physical Society meeting in emerging was ionized as it passed through the electron beam Washington, DC, in April 1939. This was only a few months 240 238 236 234 232 ATOMIC MASS UNITS Figure 3.
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