LABORATORY OF THE MONTH
Analytical Spectroscopy Aids Materials Research at AEC Laboratory at Iowa State A RAMBLING WOODEN building on the campus of Iowa State University a t Ames served as the first production plant for u r a n i u m metal during World W a r II. I t produced over 2 million pounds of the metal b y t h e end of the w a r for use i n reactors a t Chicago, O a k Ridge, and Hanford. Other activities associated with Iowa State's M a n h a t t a n Project included basic studies on t h e chemical a n d physical properties of materials essential t o the atomic energy program. Following t h e w a r t h e university established the I n stitute for Atomic Research. I t s purpose was to build up and m a i n t a i n a strong group of scientists working in t h e fundamental sciences which apply t o nuclear processes, to develop those phases of chemistry, m e t a l lurgy, physics, engineering, a n d biology associated with this field, and t o t r a i n graduate students in the science and techniques required in t h e atomic energy endeavors. In 1947 the Atomic Energy Commission established the Ames L a b o r a t o r y , a research facility which is a n integral p a r t of t h e I n s t i t u t e for Atomic Research. W i t h A E C financial support, t h e institute now consists of five modern buildings which a r e devoted t o metallurgy, metals development, and research. W i t h completion in 1963 of a 5000-kw. research reactor, A E C capital investment in the Ames L a b o r a t o r y will exceed $14 million. T h e university h a s constructed two other buildings for offices and research in chemistry, and physics, and t h e synchrotron building which houses accelerators for providing electrons or x-ray beams of 80-mev. energy. The staff totals approximately 700 of which 425 a r e scientists. The scientific group includes 200 graduate students in chemistry, physics, metallurgy, a n d engineering. University professors divide their time b e tween teaching and research supervision a t t h e institute. W i t h t h e support of graduate assistantships, more t h a n 290 scientists have received Ph.D.'s a n d over 270 their M.S.'s. T h e institute h a s been t h e source of more t h a n 1100 published scientific papers. T h e present institute programs are centered around basic research on the chemistry, metallurgy, and solid state physics of the r a r e - e a r t h elements, y t t r i u m , t h o rium, and other metals and alloys. Special emphasis is placed on metal systems which show promise in v a r i ous aspects of converting nuclear energy into useful power. I n recent years, all of the naturally-occurring rare earth elements have been prepared in metallic form and the properties of t h e pure metals and their alloys explored. Over 18,000 pounds of y t t r i u m metal was produced during the 1956-58 period.
The analytical applications of vacuum ultraviolet spectra of atoms and molecules excited in electrodeless discharge tubes of various types are studied with this apparatus
T h e successful development of chemical processes for producing pure metals from the available raw m a terials requires accurate analytical information in each step. A t t h e institute, this information is provided by the Analytical Chemistry and Spectrochemistry Sections. Although these sections operate as independent units in separate buildings, their efforts are closely coordinated. T h e Spectrochemistry Section, with a total manpower of 24, is equipped t o conduct fundamental research in spectroscopy as well as to perform analyses on a large variety of samples. A p proximately 10,000 samples per y e a r are examined or analyzed b y optical emission, x-ray fluorescence, infrared absorption, optical fluorescence, a n d electron microprobe techniques. VOL.
34, NO. 1, JANUARY 1962
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87 A
LABORATORY OF THE MONTH
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A versatile, direct-reading spectrograph is used for research studies requiring maximum precision in the measurement of intensity ratios
The characteristics and analytical applications of electrical discharges in atmospheres other than air are under systematic study. These have led to the development of an optical emission spectrometric technique for determining oxygen, nitrogen, and hydrogen in metals
An electron microprobe is used to determine the composition of 1 square micron areas of metallic inclusions, precipitated phases, diffusion zones, and other nonhomogeneous distributions in metallic systems 88 A
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ANALYTICAL CHEMISTRY
OUTSTIRS OUTLASTS OUTSELLS A new approach to the determination of the combined oxygen and nitrogen content of metals is based on extracting these elements as CO and N 2 with a high current d-c carbon arc discharge in pure helium. After extraction, a portion of the gas mixture is analyzed gas chromatographically
Optical emission spectroscopy provides a large part of the analytical data required by the Ames Laboratory. The analysis of rare earth mixtures, purity determinations on separated rare earths, and the analysis of zirconium-hafnium mixtures are typical examples. Because of the non-routine nature of most of the analyses, photographic recording is commonly used
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Aside from the usual applications of infrared spectroscopy, the frequency shift caused by N 15 substitution into nitrogen-containing compounds is employed to characterize absorption bands arising from nitrogen motion in the molecule. A microscope attachment is used to observe spectra of small crystals
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3 4 , N O . 1 , JANUARY
1962
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89 A