News and Views
Analytical Division, ACS, Meets in Atlantic City, N.J. September 8 - 1 3 , 1974 Convention Hall
More than 100 papers will be pre sented at the Analytical Chemistry Division sessions at the fall National American Chemical Society Meeting. In addition to general papers, there are symposia on educational and sci entific progress in forensic science (joint with the Division of Chemical Education), spectroelectrochemistry, analytical methods in oceanography, recent developments in bio-organic
mass spectrometry, preparative scale chromatography, and analysis of sur faces and concentration profiling in depth. All sessions will be held in the Convention Hall which will also house the exposition of latest chemicals, equipment, publications, and services. In conjunction with the meeting, the ACS will be holding short courses on technical and scientific writing, carbon-13 NMR spectroscopy, man
agement of technology, thermal meth ods of analysis, and molecular photo chemistry of organic molecules. See Short Courses, ρ 802 A, for informa tion on those courses related to ana lytical chemistry. The June 24 issue of Chem. Eng. News contains detailed information on registration, housing, and other plans. The August 5 issue will contain complete program information.
PROGRAM
10:20 Introductory Forensic Science Course in Law Enforce ment Program. R. Saferstein, New Jersey State Police 10:50 Graduate Education and Research in Forensic Chemistry. B. L. Karger, Northeastern Univ. 11:30 LEAA's Forensic Science Research Program. J. L. Peterson, Law Enforcement Assistance Admin istration, Washington, D.C.
teins. L. Mackey, Y. Fujihira, T. Ku wana, Ohio State University; C. R. Hartzell, Pennsylvania State Univ. 10:45 Spectroelectrochemistry of Cytochrome Electron Transfer Reactions. G. S. Wilson, M. D. Ryan, Univ. of Arizona 11:25 Spectroelectrochemical Studies of Metalloporphyrins on Microsecond Time Scale. N. Winograd, D. H. Karweik, Purdue Univ.
Section Β
Monday Afternoon
Symposium on Spectroelectrochemistry
Section A
Division of Analytical Chemistry G. H. Morrison, Chairman F. A. Guthrie, Secretary R. A. Osteryoung, Program
Chairman
MONDAY, SEPT. 9 Monday Morning Section A
Symposium on Educational and Scientific Progress in Forensic Science {Joint with Division of Chemical Education, Inc.)
G. Davies, Presiding 9:10 Forensic Science Education— A Perspective. R. F. Turner, Michi gan State Univ. 9:40 Educators in Forensic Science: Men in the Middle. W. McGee, FTU Forensic Science Teach ing Lab, Fla.
T. Kuwana, Presiding 9:05 Protonation of a Quinone Radical Anion. J. N. Burnett, David son College; R. M. Wightman, R. W. Murray, Univ. of North Carolina 9:35 Nucleophilic Addition Reac tions of EE Systems. J. F. Evans, H. N. Blount, Univ. of Delaware 10:15 Spectroelectrochemical Evaluation of E°' Values and Ki netic Parameters of Heme Pro
^^_
Symposium on Educational and Scientific Progress in Forensic Science (Joint with Division of Chemical Education, Inc.)
B. L. Karger, Presiding 2:00 The Application of Materials Science Methods to Forensic Prob lems. B. C. Giessen, D. Polk, Northeastern Univ. 2:30 Forensic Applications of Scanning Electron Microscope. G.
A N A L Y T I C A L CHEMISTRY, VOL. 46, NO. 9, AUGUST 1974 · 791 A
News and Views
Judd, Rensselaer Polytechnic Insti tute; J. Sabo, S. Ferriss, New York State Police Scientific Lab 3:00 Recent Developments in Bul let Search Systems. A. Johnson, New York City Police Dept. 3:30 Progress in Firearm Residue Detection. E. Rudzitis, Illinois Bu reau of Identification, Joliet, 111.; M. Wahlgren, ANL, Argonne, 111. 4:00 Gunshot Residue: Neutron Activation Analysis and Atomic Absorption Spectrophotometry... A Comparison. W. D. Kinard, D. R. Lundy, U.S. Treasury Dept., Wash ington, D.C. 4:30 Recovery and Identification of Residues of Flamable Liquids from Suspected Arson Debris. C. E. Yates, Jr., FBI Lab, Washington, D.C. Section Β
Symposium on Spectroelectrochemistry T. Kuwana, Presiding 2:00 Resonance Raman Spectro electrochemistry. D. L. Jeanmaire, R. P. Van Duyne, Northwestern Univ. 2:35 Reflection Spectroscopy of Chemisorbed Monolayers. J. D. E. Mclntyre, W. F. Peck, Jr., Bell Labs 3:05 Spectroscopic Observation of Adsorption on Thin-Film Elec trodes. W. N. Hansen, Utah State Univ. TUESDAY, SEPT. 10 Tuesday Morning Section A
Symposium on Educational and Scientific Progress in Forensic Science (Joint with Division of Chemical Education, Inc.) B. C. Giessen, Presiding 9:00 Forensic Applications of Dif ferential Scanning Calorimetry. J. H. Hall, B. Cassel, Perkin-Elmer Corp. 9:30 Ink Analysis—Weapon Against Crime and in Detection of Fraud. R. L. Brunelle, A. A. Cantu, Bureau of ATF 10:00 Forensic Bloodstain and Physiological Fluid Analysis. R. C. Shaler, W. C. Stuver, Pittsburgh and Allegheny County Crime Lab
10:30 Effect of Environmental Factors on Starch Gel Electrophoretic Patterns of Human Erythro cyte Acid Phosphates. C. G. McWright, J. J. Kearney, J. L. Mudd, FBI, Washington, D.C. 11:00 Comparison of Heroin Sam ples. S. P. Sobol, A. R. Sperling, Drug Enforcement Administration 11:30 Tissue Concentration of Morphine in Opiate-Related Deaths. L. A. Dal Cortivo, Office of the Medical Examiner, N.Y.; M. Cefola, Fordham Univ. 12:00 New Applications of Lumi nescence Techniques in Forensic Chemistry. P. F. Jones, The Aero space Corp. Section Β
Symposium on Analytical Methods in Oceanography T. R. P. Gibb, Jr., Presiding 9:05 Fundamental Problems in Océanographie Analysis. D. N. Hume, MIT 9:50 Mercury Analysis in Seawater Using Cold-Trap Preconcentration and Gas-Phase Detection. W. F. Fitzgerald, Univ. of Connecticut 10:05 Automated Anodic Stripping Voltammetry of Zn, Cd, Pb, and Cu in Seawater. A. Zirino, S. H. Lieberman, Naval Undersea Center, San Diego 10:25 Apparatus for In-Situ Concentration of Trace Metals from Seawater. E. W. Davey, A. Soper, National Marine Water Quality Lab, R.I. 10:40 An Evaluation of A P D C / MIBK Extraction System for Trace Metals in Seawater. R. J. Stolzberg, T. R. Gilbert, A. M. Clay, K. V. Ladd, New England Aquarium Central Wharf 11:00 Analytical Procedures for Transuranic Elements in Seawater and Marine Sediments. H. D. Livingston, V. T. Bowen, D. R. Mann, Woods Hole Océanographie Institution 11:20 Determination of Transition Metals in Aqueous Solution by APDC Chelate Coprecipitation. E. Boyle, J. M. Edmond, MIT 11:40 Collection and Analysis of Radionuclides in Seawater. W. B. Silker, Battelle-Northwest Tuesday Afternoon
2:30 Shipboard Determinations of CO and C1-C4 Hydrocarbons in the East Tropical Pacific. R. A. Lamontagne, J. W. Swinnerton, W. D. Smith, Naval Research Lab 2:50 Sedimentary Fluorite in Tampa Bay, Fia. W. H. Taft, D. F. Martin, Univ. of South Florida 3:10 Sampling and Analysis of Nonvolatile Hydrocarbons in Ocean Water. R. A. Brown, J. J. Elliott, J. M. Kelliher, T. D. Searl, Esso Research & Engineering Co. 3:30 Methods for Collection of Marine Samples for Trace Organic Analysis. G. R. Harvey, W. G. Steinhauer, D. H. Stuermer, Woods Hole Océanographie Institution 4:00 Aromatic Hydrocarbons Found in a Highly Anoxic Sediment. R. A. Hites, W. Biemann, MIT 4:30 Analysis of Organic Carbon in Seawater. P. J. Wangersky, Dalhousie Univ., Canada Section Β
General C. L. Wilkins, Presiding 2:00 Hadamard Transform Carbon-13 NMR Spectra. Pattern Rec ognition Analysis. R. R. Brunner, R. C. Williams, C. L. Wilkins, P. J. McCombie, Univ. of Nebraska-Lin coln 2:20 Determination and Applica tion of X-ray Diffraction Refer ence Intensities. F. H. Chung, Sher win-Williams Research Center 2:45 Study of the MECA Spectros copy of Chloride, Bromide, and Io dide in Presence of Indium. R. Belcher, S. L. Bogdanski, A. Townshend, Univ. of Birmingham, UK; D. A. Stiles, Acadia Univ., Canada 3:10 Direct Titration of WaterSoluble Sulfide in Estuarine Muds. E. J. Green, D. Schnitker, Univ. of Maine 3:40 Design of Specialized Resins for Trace Analysis. D. S. Hackett, S. Siggia, Univ. of Massachusetts 4:05 Effect of Na+ and M g + + on Carbonate Titration Curves. M. R. Kamal, G. O. Pierson, M. Sharaf, Col lege of Petroleum & Minerals, Saudi Arabia WEDNESDAY, SEPT. 11 Wednesday Morning
Section A
Section A
Symposium on Analytical Methods in Oceanography
Symposium on Analytical Methods in Oceanography
T. R. P. Gibb, Jr., Presiding 2:00 Gas Chromatographic Mass Spectrometry. Principle and Interpretation. K. Biemann, MIT
T. R. P. Gibb, Jr., Presiding 9:00 Acid-Base Measurements in Seawater. R. G. Bates, University of Florida
792 A · ANALYTICAL CHEMISTRY, VOL. 46, NO. 9, AUGUST 1974
9:35 Seawater Nutrient Analyses. P. K. Park, Oregon State Univ. 9:55 Advances in Applications of Heated Graphite Atomizer Flameless Atomic Absorption in Ocean ography. D. A. Segar, National Oce anic & Atmospheric Admin., Fla. 10:25 Comparisons of Sample Contamination by Pumping Sys tems, Niskin Bottles with Rubber and Teflon-Coated Coil Springs, and N e w Niskin Bottles Without Internal Closures. D. A. Segar, G. A. Berberian, NOAA/AOML, Fla. 10:40 Comparison of Heterogene ous Solution Rate Constants of Acid-Cleaned Biogenic Silica with Naturally Decomposing Phytoplankton Cultures. D. C. Hurd, J. M. Olmon, Univ. of Hawaii 11:10 In-Situ Sampling Tech niques for Trace Analysis in Water. H. B. Mark, Jr., K. E. Paulsen, R. J. Boczkowski, Univ. of Cincinnati
Section Β
Symposium on Recent Developments in Bio-Organic Mass Spectrometry K. Biemann, Presiding 9:00 High-Precision Stable Iso tope Ratio Measurements from Submicrogram Samples of Organic Compounds. J. M. Hayes, D. A. Schoeller, G. E. von Unruh, Indiana Univ. 9:50 Atmospheric Pressure Ion ization (API) Mass Spectrometry. A Continuous Flow Liquid Chromatograph-Mass SpectrometerComputer (LC-MS-COM) Analyti cal System Based on API Mass Spectrometry. E. C. Horning, D. I. Carroll, I. Dzidic, M. G. Horning, R. N. Stillwell, Institute for Lipid Re search, Houston 10:40 Principles and Technique of Field Desorption Mass Spectrome try. D. A. Brent, Burroughs Wellcome Co.,N.C. 11:20 Biomedical Applications of Field Desorption Mass Spectrome try. C. C. Sweeley, J. N. Gerber, B. Soltmann, J. F. Holland, Michigan State Univ.
Wednesday Afternoon Section A
Symposium on Recent Developments in Bio-Organic Mass Spectrometry K. Biemann, Presiding 2:00 Study of Compounds of BioOrganic Interest by Field Desorp
tion Mass Spectrometry. K. L. Rinehart, Jr., R. T. Hargreaves, J. C. Cook, Jr., R. M. Milberg, K. L. Olson, Univ. of Illinois, Urbana 2:35 Accurate Mass Measurement of Ions Produced by Field Desorp tion Mass Spectrometry Using Peak Matching. C. N. McEwen, A. G. Bolinski, Du Pont 3:00 Electrohydrodynamic Ioniza tion for the Mass Spectrometry of Liquids. D. S. Simons, B. N. Colby, C. A. Evans, Univ. of Illinois, Urbana 3:35 Gas Chromatography-Mass Spectrometry on Shipboard. K. L. Rinehart, Jr., R. D. Johnson, J. C. Cook, Jr., Univ. of Illinois, Urbana 4:10 Amino Acid Sequencing of Peptide Mixtures by Gas Chroma tography-Mass Spectrometry Using Perfluoroalkylated Oligo peptide Derivatives. H. Nau, K. Biemann, MIT 4:35 Thermogravimetric Analy sis/Mass Spectrometry: Use of Combination Technique for Deter mination of Polymer Decomposi tion Mechanisms. R. G. Beimer, E. M. Chait, Du Pont, Monrovia Section Β
General H. Blount, Presiding 2:00 Kalman Filter in Analytical Instrumentation: Anodic Stripping Analysis. P. F. Seelig, H. N. Blount, Univ. of Delaware 2:20 Glass-Immobilized 8-Hydroxyquinoline for Separation of Trace Metals from Base Electrolytes Used for Anodic Stripping Analy sis. E. D. Moorhead, P. H. Davis, Univ. of Kentucky 2:40 Pulse Polarographic Analysis of Sulfide and Iodide. J. Turner, R. Abel, R. A. Osteryoung, Colorado State Univ. 3:00 Quadrivalent Antimony and Electroreduction of Antimony(V). D. C. Thornton, J. Jordan, Penn. State Univ. 3:20 Measurement of Enzyme E° ' Values by Optically Transparent Thin-Layer Electrochemical Cells. W. R. Heineman, B. J. Norris, J. F. Goelz, Univ. of Cincinnati 3:50 Trace Analysis of Organomercury Compounds: Dependence of Quantitative Recovery on Tem perature of Wet Oxidation. D. Bris tol, P. Graven, J. Sell, North Dakota State Univ. 4:00 Instrumental Design for Pulse Injection Analyses of Mercu ry Vapor in Air. G. Dowd, G. Corte, J. L. Monkman, Environ. Health Cen tre, Canada
News and Views
THURSDAY, SEPT. 12 Thursday Morning Section A
Symposium on Preparative Scale Chromatography E. Grushka, Presiding 9:00 Continuous Modes of Chro matography: A Review. M. V. Sussman, R. N. S. Rathore, Tufts Univ. 9:25 Optimum Design Variables for Production-Scale Gas Chromatograph. J. R. Conder, Univ. College of Swansea, UK 9:50 Sequential Chromatographic Equipment for Separation of Wide Range of Organic Mixtures. P. E. Barker, R. E. Deeble, Univ. of Aston in Birmingham, UK 10:15 Advances in Design and Op eration of Large-Scale Gas Chro matographic Units. J. L. Duran, G. Hagenbach, P. Valentin, B. Roz, G. Guiochun, Ecole Polytechnique, Paris 10:40 High-Speed Liquid Chroma tography and Gas-Liquid Chroma tography Applied to Purification of Polar Pesticide Plant Metabolites. G. G. Still, E. R. Mansager, State Univ. Station, Fargo 11:00 Preparative Gas Chroma tography in Industrial Rubber Laboratory. J. B. Pausch, B. F. Goodrich R&D Center, Brecksville 11:20 Packing of Columns in Pre parative Gas Chromatography. C. E. Reese, E. Grushka, Hoffman-La Roche Inc. 11:40 Plate Model of Preparative Gas Chromatography Separation of Binary Mixtures. K. I. Sakodynsky, I. N. Rozhenko, V. Yu. Zelvensky, S. A. Volkov, Karpov Inst, of Physical Chem., Moscow
Thursday Afternoon Section A
Symposium on Preparative Scale Chromatography E. Grushka, Presiding 2:00 Applications of Preparative LC to Natural Products. J. M. Tabak, K. Nakanishi, Columbia Univ.
A N A L Y T I C A L CHEMISTRY, VOL. 46, NO. 9, AUGUST 1974 · 795 A
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4:00 High-Capacity Liquid Chro matography with Polymeric Adsor bents. D. H. Freeman, Univ. of Mary land; R. Schaffer, A. Cohen, W. E. May, National Bureau of Standards 4:20 Macromolecular Separations by Preparatory Scale Gel Perme ation Chromatography. A. R. Coo per, Dynapol, Palo Alto; A. J. Hughes, J. F. Johnson, Univ. of Conn. 4:40 Preparative LC Using MicroParticles. J. M. Attebery, K. E. Conroe, Waters Assoc.
Section Β
OmniScrihe Here are five versions of the
60434
2:25 Recycle in Preparative Liq uid Chromatography. K. E. Conroe, Waters Assoc. 2:50 Analytical and Preparative Chromatography of Metalloporphyrins on Polyamide Media. T. S. Srivastava, T. Yonetani, Univ. of Penn. 3:15 Methods Development and Related Applications of HighSpeed Preparative Liquid Chroma tography. J. P. Larmann, D. R. Baker, R. C. Williams, Du Pont 3:40 Roleof"Thruput"inHighPerformance Preparative Liquid Chromatography. K. J. Bombaugh, P. W. Almquist, Tracor, Inc.
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Symposium on Analysis of Surfaces and Concentration Profiling in Depth W. L. Harrington, Presiding 9:05 In-Depth Analysis of Solid Surfaces by Low-Energy Ion Scat tering Spectrometry. W. L. Harring ton, RCA Labs 9:45 Ion Microprobe Analysis of Surfaces and Thin Films—Advan tages, Limitations, and Applica tions. J. A. McHugh, General Electric Co. 10:35 Materials Characterization by Auger Electron Spectroscopy and Secondary Ion Mass Spectrom etry. J. M. Morabito, Bell Telephone Labs 11:15 Polymer Surface Analysis Using ESCA. W. M. Riggs, Du Pont, Monrovia
FRIDAY, SEPT. 13
Section Β
Symposium on Analysis of Surfaces and Concentration Profiling in Depth
Friday Morning General—Chromatography
W. L. Harringtn, Presiding 2:00 Measurement of Concentra tion Profile of Boron Implantations in Silicon by Secondary Ion Mass Spectrometry. W. Hofker, Philips Res. Lab, Eindhoven 2:40 In-Depth Elemental Analysis of Thin Films by Glow Discharge Mass Spectrometry. J. W. Coburn, IBM, San Jose 3:30 Surface Studies of Electronic Devices with AES and SLEEP Techniques. H. F. Gray, G. A. Haas, Naval Res. Lab 4:10 Surface Analysis of Metals and Metal-Oxides Using ESCA. N. Winograd, K. S. Kim, Purdue Univ.
Timothy Nieman
P. C. Jurs, Presiding 9:00 Determination of Crude Oil Type from Gas Chromatograms Using Pattern Recognition Tech niques. H. A. Clark, P. C. Jurs, Penn. State Univ. 9:20 Detection and Estimation of Low Levels of Dimethyl Sulfide in Isoprene by Gas Chromatography (FPD). J. E. Sanders, Goodyear Tire & Rubber Co. 9:40 In-Situ Chemically Bonded Stationary Phases for High-Pres sure Liquid Chromatography. I. Optimization and Evaluation. R. K. Gilpin, J. A. Korpi, C. A. Janicki, McNeil Labs
Stephen Wise
Michael McConnell
10:00 High-Performance Liquid Chromatography of Fatty Methyl Esters: Preparative Separations. C. R. Scholfield, Northern Regional Res. Center, Peoria 10:20 Plot Columns Combined with Packed Precolumns. J. G. Nikelly, Phila. College of Pharmacy & Science 10:50 Some Further Applications of Alkali Fusion Reaction Gas Chromatography to Organic Func tional Group Analysis. D. D. Schlueter, S. Siggia, Univ. of Mass. 11:10 Thermodynamic Selection Criteria for Liquid Phases in GasLiquid Chromatography: Nonempirical Approach. B. L. Reinbold, T. H. Risby, Penn. State Univ. 11:30 Selective Separations by Reactive Ion Exchange (RIEX). G. E. Janauer, G. O. Ramseyer, J. W. Lin, SUNY-Binghamton
Brian Renoe
Thomas Cook
1974 Fellowship Awards
Terry Woodruff
Richard Winslow
The Fellowship Committee of the Division of Analytical Chemistry, American Chemical Society, has an nounced the winners of its full-year awards for 1974. Two awards of $5000 have been made. Timothy Alan Nieman of Michigan State University won the award spon sored by the Procter & Gamble Co. He is working with C. G. Enke. Mr. Nie man wishes to develop a computer in terfaced vidicon spectrophotometer system, to make use of the vidicon spectrometer's ability to record com plete spectra in a short amount of time (33 msec), to study the kinetics of the chemiluminescent reaction of luminol. The Perkin-Elmer Corp. fellowship has been awarded to Stephen Albert Wise of Arizona State University. His supervisor is Richard S. Juvet, Jr. He
is working on the theoretical and prac tical development of a new, ultra-sen sitive, universal detector for liquid chromatography, the flame aerosol de tector (FAD). Five winners of $800 summer fel lowships have been named. Michael Lowe McConnell, working with Milos V. Novotny at Indiana University, has won the award by Carle Instruments, Inc. His research is on the design and development of an automated system for the gas chromatographic separa tion and analysis of the volatile con stituents of body fluids. The fellow ships sponsored by Olin Corp. Chari table Trust were awarded to Brian William Renoe of the University of Il linois and Thomas Edward Cook of Purdue University. Mr. Renoe, work ing with H. V. Malmstadt, is doing a computer study of the use of a centrif-
A N A L Y T I C A L CHEMISTRY, VOL. 46, NO. 9, AUGUST 1974 · 797 A
ugal fast analyzer in clinical chemis try. Mr. Cook is working with H. L. Pardue on the evaluation of the vidicon and related tubes as detectors for atomic spectroscopy. These analyses will be based upon atomic emission absorption, fluorescence, and combi nations of these phenomena. The Division of Analytical Chemis try has, itself, sponsored two fellow ships again this year. Terry Alaric Woodruff of the University of Illinois and Richard J. Winslow of the Univer sity of Massachusetts were the awardees. Mr. Woodruff, working with H. V. Malmstadt, is doing his research on
the development of a computer-con trolled, automated instrument for the accurate determination of trace ele ments in environmental and clinical samples. This instrument will be used for basic studies of the atomic vapor produced by the pulsed arc source. Mr. Winslow is working with Ramon M. Barnes on a study of the processes associated with a low-temperature plasma ashing. This recipient will in vestigate heterogeneous and homoge neous reaction mechanisms occurring in the ashing of solid substances with a low-temperature, low-pressure reac tive plasma.
Process Instrument Justification Manpower savings Safety Government regulation Increased control (specification p r o d u c t i o n ) Increased t h r o u g h p u t Reduced down-time Raw material savings Source: R. A. Hagstrom, Olin Corp.
Return on Investment = , -S™s
R0|
100
Instrument Cost Consider: Instrument and installation cost and sampling system will cost $200,000 Case I
On-Line Process Instrumentation More than 125 participants heard experts give information on on-line process analytical chemistry at the ACS Analytical Chemistry Division's 27th Annual Summer Symposium at Colorado State University, June 1214. The technical discussions were opened by Sidney Siggia of the Uni versity of Massachusetts who remind ed the audience that he was saying in 1959 that analytical chemists should be more involved in process control applications, and he is still saying that today. This set the theme of the meet ing. The need for greater communica tion between the engineers, chemical and electrical, who deal with plant processes and the man in the lab was emphasized throughout. As it was stated more than once, "Don't wait in the lab for the problems to come to you; go out in the plant." Some of the attendees had done just that and were at the meeting to get information to aid in their particular processes. Richard Hagstrom of Olin Corp., who with F. W. Karasek of the Univer sity of Waterloo planned the program, gave information on how to approach on-line problems. Included in his pre sentation were factors to consider and especially justifications for on-line process control. He gave a practical example of process instrumentation justification with actual cost, sales, profit, plant capacity, down-time, and on-stream improvement figures (see tables). L. Fowler of Monsanto Indus trial Chemical Co. discussed at some length process analyzer sample prob lems. This is a key area in any on-line process control application. If the sampling problem is not solved prop erly, the measurements will not relate correctly to the process. Separate sessions were devoted to process chromatography, chaired by John Scales of Bendix; spectroscopic
Manpower savings (one man with fringes = SE0,000/yr)
R o - f i g κ™ = 30* instrumentation, chaired by W. V. Dailey of Mine Safety Appliances Co.; and electroanalytical instrumentation, chaired by F. H. Zimmerli of Rohm & Haas Co. Much of the information given was related to new consider ations involved when adapting a lab method to the line. In this endeavor, more than one speaker pointed out that one learns to be a plumber! Some specific case histories in which on-line process control was necessary were given by I. A. Capuano of Olin Corp. For example, in the production of hy drazine for space use, the plant could not be insured without proper safety consideration which involved on-line control. In this instance, the process control instrumentation (GC) was used to gain much needed information on just what was happening in the process. Capuano stressed that on-line process control should only be consid ered for problems that are important. Overall, much emphasis was placed on the need for simplicity, careful con sideration of sampling systems, "jig gling" the instrument into the particu lar application, and better communi cation between the man in the lab and the man in the plant. Representatives from instrument companies (J. Scales, Bendix Corp.; Roger LeBrand, Hewlett-Packard; W. V. Dailey, Mine Safety Appliances Co.; R. S. Saltzman, Du Pont; M. Du Gros, Technicon; R. Oliver, Foxboro Co.; H. Ross, Orion Research; L. Barnes, Milton Roy/Hays; and R. Dishman, Ionics), in discussing their particular fields and instruments, all emphasized the need for full commu nication on what is needed and why, so that a successful installation can be accomplished. In the final presentation at the sym posium, Kenneth W. Gardiner de scribed the Applied Science Program
798 A · ANALYTICAL CHEMISTRY, VOL. 46, NO. 9, AUGUST
1974
Payout in three and one-half years Case II Fifteen percent plant capacity in crease
R O I
=32S0XI
O O
=^
Payout in 20 days Case III Reduced down-time If instrument saved one down-time/year
ROI
= !oWo = 41%
Payout in 2.43 years (Now figure as a result of multiple effects) Case IV Improved on-stream factor Instrument improved on-line factor by 5%
"0.=\™^?X !«» = ««% Payout in six days Source: R. A. HaKstrom, Olin Corp.
now being developed at the University of California in Riverside as a means of improving instruction in process analytical chemistry. This program is outside the classical science depart ments and multidisciplinary in organi zation so that a teaching-training cur riculum more in keeping with "realworld" demands in the process area of instrumentation is feasible. The weather was perfect, the setting with the Rocky Mountains in the background, beautiful, and the cam pus facilities were modern and attrac tive. All the local people and especial ly Rodney Skogerboe, local arrange ments chairman, and Robert Osteryoung, chemistry department chair man, were helpful to participants. Col orado State University has a strong graduate program in analytical chem istry. The chemistry department, which is housed in a new building with extensive teaching and research facili ties, has a faculty of 28, more than 20 postdoctoral fellows, and 60-70 gradu ate students.
News and Views
The device, which is exhibiting a pronounced trace on the recorder, detects trace quantities of surfactants. A shallow water channel is formed by the two bars running diagonally across the photo. The water flows from right to left. The measuring device for surface films consists of the knife-edge barrier (arrow) placed across the channel and suspended from a torsion wire above it. Pressure of the hydrophobic film induces a torque on the wire, whose rotation is detected via a displacement transducer Film of surfactants made visible (top) with talc appears to the camera as cloudy clumps floating on the water. The photo clearly shows the upstream limits of the surface film, marked by the line extending nearly across the channel at right
Device to Measure Surfactant Concentation A novel device for measuring the concentration of surfactants in water has been disclosed by a research group at the University of Colorado in Boulder. Phillip C. Martin, a doctoral student in chemical engineering; William B. Krantz, associate professor of chemical engineering; and Walter A. Weers, associate professor of civil and environmental engineering, have developed a highly sensitive instrument for measuring the surface and bulk concentrations of hydrophobic contaminants. The operating principle of this instrument involves the phenomenon of hydrodynamic stagnation in the interface of a flowing liquid. A thin film typically 1 mm or less in thickness flows through a nearly horizontal trough. An interfacial stagnation barrier or line is created downstream by touching the flowing interface with a nonwetting rod or knife-edge placed perpendicular to the direction of flow. This initiates the growth of a "stagn a n t " layer of surfactant molecules at the interface. The interfacial stagnation line does not permit any molecules to escape by convection from the
interface. Thus, a "stagnant" film of surfactant molecules begins to accumulate in the interface. This film is stagnant in the sense that there is no convection or bulk motion of fluid within it. However, it is dynamic or growing in the sense that the length of this stagnant film will increase because of more material being converted in at its upstream edge. Its ultimate length is limited only by desorption of surfactant molecules into the bulk liquid stream, evaporation into the ambient gas phase, two-dimensional surface phase transitions, or multilayer film formation. The phenomenon of stagnation in a fluid interface has been studied in some detail for the past decade. However, most investigators have been concerned with the time growth of the film made visible by sprinkling talc particles in the interface. Whereas such studies are of definite value in elucidating the fundamentals of stagnant film growth, they do not lend themselves to a convenient measurement technique for routine analyses. Martin, Krantz, and Weers are the first investigators to suggest using the
phenomemon as a practical means to detect surfactant concentration in water. The measurement principle of their instrument relies on the fact that the "stagnant" film causes a rearrangement of the velocity profile on the bulk fluid. This effect produces a hydrodynamic drag on the "stagnant" film, resulting in a force in the interfacial stagnation barrier. The total force on the interfacial stagnation barrier can be related to the equilibrium surface and bulk concentrations of the hydrophobic contaminants when the surface equation of state, bulk-phase hydrodynamics, and adsorption-desorption characteristics of the surfactant are known. For the dilute surfactant films associated with natural water streams and tertiary effluent from a waste treatment process, the data analysis is considerably simplified since the two-dimensional ideal gas law describes the thermodynamic state of the adsorbed species, and adsorption-desorption considerations can be ignored. Bulk concentrations associated with unknown mixed surfactant monolayers can be expressed in terms of equivalent concentration
ANALYTICAL CHEMISTRY, VOL. 46, NO. 9, AUGUST 1974 · 799 A
News and Views of linear alkyl sulfonate as prescribed in the standard test methods published by the American Public Health Association. The instrument provides for the controlled hydrodynamics and continuous force measurement needed to use the principles described above. To measure these small forces, which are typically 100 dynes or less, Martin, Krantz, and Weers have developed a sensitive dynamic torsion balance. The interfacial stagnation barrier is suspended from an arm which is attached to a calibrated torsion wire. The progressive rotational displacement of this wire is detected via a displacement transducer. Although torsional devices have been in use for several years in sensitive force measurement for static Langmuir troughs, Martin, Krantz, and Weers are unaware that such devices have been adapted to semicontinuous measurement of unsteady state interfacial dynamics. The prototype device developed by the University of Colorado research group has proved quite successful relating rapid measurement of the concentration of both soluble and insoluble surfactants of varying types. In particular, the device has been used to determine the bulk-phase concentration of a colloidal polyelectrolyte which is used in tertiary waste water treatment; the instrument proved capable of detecting the polyelectrolyte concentration at the ppm level with a reproducibility of 2%. The range and sensitivity can be conveniently changed by adjusting the bulk flow rate, channel inclination, or characteristics of the torsion wire. Advantages of this instrument are its high sensitivity (
