News Analytical Chemistry Division Names Graduate Fellowship Award Winners T h e Fellowship Committee of the American Chemical Society Division of Analytical Chemistry has announced the winners of the three $5 000 full-year awards and seven $1 000 summer fellowships for 1977. Winners of the full-year awards are Steven D. Brown of the University of Washington, Grover D. Owens of Purdue University, and Richard A. Yost of Michigan State University. Steven D. Brown, whose award is sponsored by the Perkin-Elmer Corp., is working with Bruce R. Kowalski. He is currently engaged in research to develop computer-controlled techniques applicable to anodic stripping voltammetry and is particularly interested in the application of the technique to the analysis of natural geothermal effluents. Grover D. Owens' major research project, under Dale W. Margerum, involves the development of analytical techniques to observe very fast electron transfer reactions. A continuous flow instrument interfaced to a computer will be used for this study. The award is sponsored by Procter & Gamble. Richard A. Yost, whose sponsor is T h e Upjohn Co., is working with C. G. Enke on the development of a tandem quadrupole mass spectrometer with an intelligence control system to be used for the analysis of mixtures and the elucidation of the structures of organic compounds. T h e recipients of the $1 000 summer fellowships and their respective sponsors are: Christopher F. Bauer, Colorado State University, Carle Instruments, Inc.; Kelsey D. Cook, University of Wisconsin, Division of Analytical Chemistry; Michael F. Delaney, University of Massachusetts, Olin Corp. Charitable Trust; Mauri A. Dit-
zler, Duke University, Society for Analytical Chemists of Pittsburgh; John M. Ramsey, Indiana University, Olin Corp. Charitable Trust; Alexander Scheeline, University of Wisconsin, Division of Analytical Chemistry; and Lawrence F. Whiting, University of Georgia, Division of Analytical Chemistry. Christopher F. Bauer is working with David F. S. Natusch on the application of microwave plasma emission spectrometry to environmental chemistry. Kelsey D. Cook, in collaboration with James W. Taylor, is studying the problem of cluster formation and cluster dynamics in alcohols and ammonia with the aid of supersonic molecular beam photoionization mass spectrometry. Michael F. Delaney, under Peter C. Uden, is principally involved with the isolation and identification of chlorinated molecules produced by direct chlorination of humic substances by high-performance liquid chromatography by use of novel stationary phases and specific detectors developed for this project. Mauri A. Ditzler is working under the supervision of William F. Gutknecht on the elucidation of toxic particles present in materials such as fly ash. A variety of analytical techniques, including wet chemical methods and photon-induced x-ray emission analysis, are being used for the study. John M. Ramsey is working with Gary M. Hieftje. T h e thrust of his research is to determine subnanosecond events by spectrometric methods. While the technique has initially been used to measure luminescence life times, its potential in the measurement of rapid chemical kinetics and energy transfer rates is also important. Alexander
hristopher
Bauer
John
Ramsey
Alexander
Michael
Delaney
Lawrence
Mauri
Scheeline
Whiting
Ditzler
Correction
Steven Brown
Grover Owens
Richard Yost
The 1977 Chemical Instrumentation Award is administered by the Division of Analytical Chemistry. The administering organization is incorrectly identified in the J u n e issue, page 605 A.
ANALYTICAL CHEMISTRY, VOL. 49, NO. 8, JULY 1977 ·
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News
THE LC COLUMN July/August New Zorbax-CN for both normal and reversedphase HPLC. T h e new Z o r b a x - C N m i c r o p a r ticular c o l u m n , with c h e m i c a l l y bonded cyano phase, is effective for separations in both normal and reversed-phase partition HPLC.
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A third example shows the same column demonstrating unique selectivity in a separation of drugs Figure 3 Column: Zorbax-CN Mobile Phase: 15% IPA/ 85% Hexane PEAK IDENTITY 1. 3-lsobutylmethylxanthene
University of Akron Professor Honored
2. Caffeine 3. Chloramphenicol
Figure 1
4. Cortisol
-^
Column: Zorbax-CN MINUTES 0
Mobile Phase: 0.1% Propionic Acid 1 % Heptane Sulfonic Acid Sodium Salt, 98.9%H,0
1. 2. 3. 4. 5.
uracil Thymine Cytosine Guanine Adenine
MINUTES 0
For example, a rapid reversedphase separation of key nucleic acid bases is easily achieved on Zorbax-CN. (Figure I) Analysis of these bases is critical in studies of proteins and polypeptides.
1
Figure 2 Column: Zorbax-CN Mobile Phase: 5% CR.CN 95% 0.1 M
3
NaOAc pH 4.6 PEAK IDENTITY
|4 2
1 .Vanilmandelic Acid 2. Epinephrine 3. Metanephrine 4. Homovanillic Acid
ΙΟ
in the normal partition mode. (Fig ure 3) Note that there are no inter ferences. Coextractants which would often be retained on a silica a d s o r b e n t are not r e t a i n e d o n Zorbax-CN under these conditions.
PEAK IDENTITY
r
MINUTES 0
0
5
,
In another example, a rapid analysis for several critical members of the catecholamine family is developed on Zorbax-CN. (Figure 2) These compounds play a key role in nerve system conduction.
Scheeline, working with John P. Wal ters, is interested in the phenomena involved in transient electrical dis charges of atomic systems. Lawrence F. Whiting is working on the DSC modification as applied to enzymesubstrate characterization. Under Peter W. Carr, he is developing a working error guideline for kinetics in DSC by using the orthogonal collo cation method of simulation.
Paul D. G a m , professor of chemis try at the University of Akron, Ohio, has been named to receive the 1977 Du Pont Award from the Internation al Confederation for Thermal Analysis (ICTA). T h e award, consisting of a $1000 honorarium and trip expenses, will be presented to Dr. Garn at the
Zorbax-CN columns, as well as all Zorbax columns, are quality control tested by DuPont before shipment, and guaranteed to perform to spec ifications. For more information cir cle reader service card 49.
Zorbax15cm columns: the short and the long of it. Du Pont Instruments' Zorbax-SIL, Zorbax-ODS and Zorbax-CN ana lytical columns are available in a 4.6 m m ID χ 15 c m configuration. Although short in length, they are long in performance, offering very good resolution at low back pres sures—typically less than 1,000 psi. This means improved performance with less maintenance for dedi cated HPLC units used in quality control applications. The price is advantageous, t o o . . . $ 2 0 0 for the Zorbax-ODS column, for example. For more i n f o r m a t i o n , circle the reader service card or write DuPont Instruments, Room 35836, Wilmington, DE 19898.
Du Pont Instruments CIRCLE 49 ON READER SERVICE CARD 704 A · ANALYTICAL CHEMISTRY, VOL. 49, NO. 8, JULY
1977
Paul D. Garn 5th ICTA Conference in Kyoto, Japan, August 1-6, 1977. At the con ference he will present an award lec ture on the kinetic parameter. Dr. G a m ' s experience and research in thermal analysis began in 1948 with his master's degree work and contin ued through his work with Bell, where he developed techniques for measur ing capacitor stabilizing additives and alkyl resin components. His research interests at the University of Akron since 1963 have included the develop ment of thermoanalytical methods, ki netics of thermal decomposition, mechanisms of solid-solid transitions, calorimetry and thermodynamics of the liquid-crystalline smectic mesomorphs, and gas chromatographic methods. Dr. Garn is the first recipient of the award, which is sponsored by Du Pont Instruments, Scientific and Process Division. T h e award will be given every three years at subsequent ICTA conferences in recognition of out standing contributions in thermal analysis.
News
Our new HPLC Columns ore well pocked!
Analytical Chemistry at Work
Guaranteed peak symmetry and minimum plates per meter doubly assure you of optimum column performance. A completely new line of "stateof the-art" packed columns for high pressure liquid chromatography is now available in the U.S. and Canada from Rheodyne. All columns are 4.6 mm ID χ 25 cm long. Each column is tested and supplied with its own chromatogram. Currently six columns are available over a price range of $180 to $240. The table below showing column performance specifications and typical test conditions offers an excellent argument for the addition of these columns to your HPLC equipment. TYPEMN Particle
SI-100· 5 μΓη
Min. plates per meter
36,000
Max. peak asymmetry
1 6
Solvent 2ffi. ml/mm Pressure, pst
NH 2 , 0 μχη 14,000 1 6
DIOL 1 0 ltm
" ..
RP-8 5 μΓη
26.000 1 6
hexane
hexane
hexane
^tonltrife"
2.0
2.0
2.0
2.0
1640
280
280
Test nitronitronitrosubstance benzene benzene benzene 'available in 10 μπι particle size also, "under evaluation
Portable S y s t e m for Clinical and Environmental Determinations A portable microprocessor-con trolled centrifugal fast analyzer (CFA) has been developed and demonstrated by a group of scientists at Oak Ridge National Laboratory. With this in strument, the composition of up to 16 different chemical and biochemical samples can be determined simulta neously within seconds. A prototype of the instrument was shown at the Ninth Annual Symposium on Ad vanced Analytical Concepts for the Clinical Laboratory held in March of this year. The centrifuge, which rotates at speeds up to 4000 rpm, forms the basis of this instrument as well as its prede cessor developed in 1968. Measure ments are made of the optical proper ties of material such as their transmis sion, fluorescence, light scattering, or luminescence. Carried out simulta neously at 17 different locations on the rotor, these measurements are compared with the known optical properties of reference materials to provide the determinations. A battery pack or 110-V alternating current provides power. T h e self-con
tained microprocessor controls the an alytical functions and provides versa tility in operating conditions, as well as acquiring and analyzing the data. Analytical options include the deter mination of reaction rates by linear re gression analysis. Applications of the instrument in mobile laboratories, in small clinics, or even at a patient's bedside are sug gested. Possibilities also exist for its use in assaying environmental pollu tants such as phosphate, silica, and ammonia. Because of its capabilities in determining reaction rates, the sys tem could be used in research investi gations of fast chemical and biochemi cal reactions. Routine clinical measurements, such as glucose, protein, or uric acid, as well as enzyme activity assays, can be handled with this system with im proved performance over earlier mod els of the miniature CFA. Work con tinues to provide computer software enabling the instrument to supply op tical measurements at multiple wave lengths during a single analysis, and for electronic self-checking by the computer. The research on this system is spon sored by the Energy Research and De velopment Administration, EPA, NASA, and the National Institutes of General Medical Sciences. The many people who contributed to the devel opment include J. E. Mrochek, C. A.
3000
diethyl phthalate
Made by Brownlee Labs, the columns are guaranteed by both Brownlee and Rheodyne. Column packings are LiChrosorb (a registered T.M. of E. Merck Darmstadt Germany). For More Information. A detailed technical brochure is available for the asking. Address Rheodyne, Inc., 2809 Tenth Street, Berkeley, CA 94710. For even faster service, phone (415) 548 5374.
RHCODSJNC
John E. Mrochek holds the rotor housing of the portable centrifugal fast ana lyzer. The instrument is 18 X 11 X 12 in. in size and weighs only 55 lb. An in corporated microprocessor controls the drive system, rotor speed, and clutchbrake and automatically synchronizes these functions with data acquisition. Other analyzer functions under microprocessor control include the selection of preamplifier gain, transmission filters, and primary and secondary filters for fluorescence
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News
Squeeze Play Tem-Pres Pressure Intensifiers
Research engineers at Detroit Edison Co. are shown with a model of the company's 3 2 0 0 - M W Monroe, Mich., plant, the world's largest coal-fired electric generating plant. Records are made of the smoke plumes from the model chimneys. This is part of the laboratory work at Detroit Edison where a full complement of sophisticated analytical in strumentation is used for the analyses of air, water, fuels, and materials
Burtis, W. F. Johnson, M. L. Bauer, D. G. Lakomy, R. K. Genung, and C. D. Scott. Details of the instrument de sign, operating characteristics, and an alytical capabilities are reported in a paper scheduled for publication in the September issue of Clinical Chemis try.
Centrifuge/ Spectrophotometer Combination William C. Deal, Jr., professor of biochemistry, and Jason Wei, postdoc toral fellow at Michigan State Univer sity, have developed an improved farultraviolet scanning ultracentrifuge. The machine's optical system and de tector, controlled by computer, is ca pable of using ultraviolet light of ex tremely short wavelengths (in the 200-nm range). For light absorption studies aimed at understanding mo lecular structure, interactions, and composition, the new system is 10-20 times as sensitive as conventional ultracentrifuges. The apparatus provides a valuable tool to study the structures of pro teins. Quantities of material as small as fractions of a microgram can be an alyzed and assayed. Spinning at 60 000 rpm, one to five samples are automatically exposed to a light beam.
A computer controls the beam and de tector, and automatically records within a few microseconds light ab sorption and numerical and graphic data. Design and construction of this in strument has been a five-year project, funded by the National Science Foun dation. Experiments that once re quired hours can now be performed in minutes, with more accurate results.
Market Study Predicts Heavy Growth in Separations In a new study published in April of this year, Creative Strategies, Inc., predicts that demands for environ mental monitoring, clinical lab testing, and research and development will provide a worldwide market for ana lytical and process analytical instru mentation of $2.1 billion by 1981. The separation market, with an average annual compound growth rate of 15%, is predicted to overtake the currently strong spectrometer segment by 1981. The impact of microprocessors will be such that by 1981 more than 60% of sales in analytical instrumentation will incorporate this technology. Beckman, Perkin-Elmer, and Varian Assoc, account for 26% of the worldwide mar ket in this industry which is character ized by fragmentation and much com petition according to CSI.
The compact Tem-Pres inlensilier. originally designed lor laboratory use. occupies minimum Moor space. The sell-contained unit automatically accepts low-pressure gas Irom an external source and compresses it to elevated pressures. Gauges indicating hydraulic drive pressure as well as inlet and intensified gas pressures are mounted on the cabinet panel. Tem-Pres constructs the units ol high-yield, vacuum-melt steel lorging. heattreated to exacting specifications.
specialists in high pressure/high temperature research systems
contact R. M Shoff
Leco Corporation T e m P r e t Division 1401 South Λιη*ποη Street Stat· Colleo·. Pennsylvania 16801 Pnona 814 237 7831
LECO CIRCLE 125 O N READER SERVICE CARD
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