MARCH 15, 1993 VOLUME 65 NUMBER 6 * >
ANCHAM Tht Audit 65(6) 279A-326A/665-848 (1993) eurtau | S S N 0003-2700
®
Analytical
CHEMISTRY
Registered in U.S. Patent and Trademark Office; «Copyright 1993 by the American Chemical Society EDITOR: ROYCE W. MURRAY, University of North Carolina ASSOCIATE EDITORS: Catherine C. Fenselau, University of Maryland Baltimore County, William S. Hancock, Genentech, James W. Jorgenson, University of North Carolina, Robert A. Osteryoung, North Carolina State University, Edward S. Yeung, Iowa State University/Ames Laboratory Editorial Headquarters, research section Department of Chemistry Venable and Kenan Laboratories University of North Carolina Chapel Hill, NC 27599-3290 Phone:919-962-2541 Fax:919-962-2542 E-mail: Murray @ uncvx1.oit.unc.edu Editorial Headquarters, A-page section 1155 Sixteenth St., N.W. Washington, DC 20036 Phone:202-872-4570 Fax: 202-872-4574 E-mail: rmh96 @ acs.org Managing Editor: Mary Warner Senior Editor: Louise Voress Associate Editor: Grace K. Lee Assistant Editor: Felicia Wach Editorial Assistant: Deborah Noble
REPORT
295 A
A brief history of NMR. Over the past 40 years NMR spectroscopy h a s become invaluable in fields such as analytical chemistry, structural biology, diagnostic radiology, and materials science. Edwin D. Becker of the National Institutes of Health recounts the development of NMR methods and advances in applications to physics, chemistry, biology, and other sciences
Contributing Editor: Marcia Vogel Head, Graphics and Production: Leroy L. Corcoran Art Director: Alan Kahan Designers: Peggy Corrigan, Robert Sargent Production Editor: Elizabeth Wood Electronic Composition: Wanda R. Gordon Circulation: David Schulbaum LabGuide Managing Editor of Directories and Databases: Kathleen Strum Associate Editor: Joanne Mullican Assistant Editor: Susan Barclay Journals Dept., Columbus, Ohio Editorial Office Manager: Mary E. Scanlan Journals Editing Managers: Kathleen E. Duffy, Anne C. O'Melia, Joseph E. Yurvati Associate Editor: Lorraine Gibb Assistant Editor: Brenda S. Wooten Advisory Board: Michelle V. Buchanan, Bruce Chase, M. Bonner Denton, Joseph G. Gordon, David M. Haaland, Joel M. Harris, Timothy D. Harris, Franz Hillenkamp, Kiyokatsu Jinno, Dennis C. Johnson, Richard A. Keller, Philip D. LaFleur, Gary E. Maciel, Geraldine Richmond, Ralph Riggin, Michael Thompson Ex Officio: Joseph L. Glajch Instrumentation Advisory Panel: Anna Brajter-Toth, Raymond E. Clement, Therese M. Cotton, Norman J. Dovichi, Jack D. Henion, Mary Ellen P. McNally, John W. Olesik, DallasL.Rabenstein, J. Michael Ramsey Publications Division Director: Robert H. Marks Head, Special Publications: Anthony Durniak Head, Journals: Charles R. Bertsch
FOCUS
315 A
On the cover. FFF. As instruments for sedimentation, thermal, and flow F F F become commercially available, use of this methodology will grow. Michel Martin of the Ecole Supérieure de Physique et Chimie I n d u s t r i e l l e s (Paris) discusses applications in environmental science, p h a r m a ceuticals, polymers, biology, and particle characterization reported at FFF '92
UPCOMING RESEARCH
291 A
NEWS
293 A
Los Alamos National Laboratory scientists improve materials by laser resurfacing. · Buckyball flagellenes synthesized by researchers at University of North Carolina-Chapel Hill and Shell Development Company. · AOAC International organizes reference materials division
MEETINGS
304 A
The 205th ACS spring national meeting will convene March 28-April 2 in Denver, CO. The technical program will feature the presentation of awards to Jeanette G. Grasselli, Seymour Meyerson, James W. Jorgenson, David M. Hercules, and James R. Fair
ROOKS
312 A
Volumes on HPLC and affinity chromatography of proteins are reviewed
NEW PRODUCTS AND MANUFACTURERS' LITERATURE
320 A
ANALYTICAL CHEMISTRY, VOL. 65, NO. 6, MARCH 15, 1993 · 283 A
Analytical® CHEMISTRY ANALYTICAL CHEMISTRY (ISSN 0003-2700) is published semimonthly by the American Chemical Society, 1155 Sixteenth St., N.W., Washington, DC 20036. Second-class postage paid at Washington, DC, and additional mailing offices. Postmaster: Send address changes to ANALYTICAL CHEMISTRY, Member & Subscriber Services, P.O. Box 3337, Columbus, OH 43210. Canadian GST Reg. No. R127571347. Copyright Permission: An individual may make a single reprographic copy of an article in this publication for personal use. Reprographic copying beyond that permitted by Section 107 or 108 of the U.S. Copyright Law is allowed, provided that the appropriate per-copy fee is paid through the Copyright Clearance Center, Inc., 27 Congress St., Salem, MA 01970. For reprint permission, write Copyright Administrator, Publications Division, ACS, 1155 Sixteenth St., N.W., Washington, DC 20036. Registered names and trademarks, etc., used in this publication, even without specific indication thereof, are not to be considered unprotected by law. Subscription and Business Information 1993 subscription rates include air delivery outside the U.S., Canada, and Mexico. Canadian subscriptions are subject to 7% GST. Members
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Articles Design of a Glucose Minisensor Based on Streptavidin-Glucose Oxidase Complex Coupling with Self-Assembled Biotinylated Phospholipid Membrane on Solid Support Maja Snejdarkovâ *, Marian Rehak, and Matthias Otto
665
Amperometric and Fast Scan-Rate Cyclic Voltammetry Detection at a Microelectrode for Gel Permeation High-Performance Liquid Chromatography of Fullerenes Benoît Soucaze-Guillous, Wlodzimierz Kutner, and Karl M. Kadish *
669
Detection and Evaluation of Fragrances by Human Reactions Using a Chemical Sensor Based on Adsorbate Detection Kenji Yokoyama * andFumihiro Ebisatva
673
Robust Procedure for Calibration and Calculation of the Detection Limit of Trimipramine by Adsorptive Stripping Voltammetry at a Carbon Paste Electrode M. Cruz Ortiz *, Julia Arcos, José V. Juarros, Jesus Lopez-Palacios, and Luis A. Sarabia
678
Application of Square Wave Voltammetry to Strongly Adsorbed Quasireversible Redox Molecules James H. Reeves *, Shihua Song, and Edmond F. Bowden *
683
Membrane Model for Neutral-Carrier-Based Membrane Electrodes Containing Ionic Sites Rudolf Eugster, Ursula E. Spichiger*, and Wilhelm Simon
689
X-ray Emission Analysis of Thin Poly(3-methylthiophene) and Poly ((3 - methylthiophene)-co-[ 1 - methyl- 3 - (pyrrol -1 - ylmethyl)pyridinium]} Films. Composition, Oxidation Level, and Overoxidation Zhigang Qi and Peter G. Pickup *
696
Determination of Total Polyamines in Tumor Cells by HighPerformance Capillary Zone Electrophoresis with Indirect Photometric Detection Rulin Zhang, Cynthia L. Cooper, and Yin/a Ma *
704
Resolution of Simultaneous Kinetic Spectrophotometric Processes by Factor Analysis Andreu Cladera, Enrique Gomez, José Manuel Estela, and Victor Cerdà *
707
Digital Imaging of Atomization Processes in Electrothermal Atomizers for Atomic Absorption Spectrometry Chuni L. Chakrabarti *, Albert Kh. Gilmutdinov, and J. Craig Hutton
716
Use of Packed Column Supercritical Fluid Chromatography with Ozone-Based Sulfur Chemiluminescence Detection A. L. Howard and L. T. Taylor*
724
Enzyme-Based Fiber Optic Zinc Biosensor Richard B. Thompson * and Eric R. Jones
730
Temporal Signal Profiles of Analytical Species in Modulated Glow Discharge Plasmas F. L. King* and C. Pan
*Corresponding author
continued
735
on p. 287 A
ACS membership information: Lorraine Bowlin (202-872-4567) ANALYTICAL CHEMISTRY, VOL. 65, NO. 6, MARCH 15, 1993 · 285 A
Analytical® CHEMISTRY Editorial Information Instructions for authors of AC RESEARCH are published in the January 1 issue, p. 91. Guidelines for the INSTRUMENTATION, REPORT, ANALYTICAL APPROACH, and A/c INTERFACE features are published in the January 1 issue, p. 90. Please consult these instructions and guidelines prior to submitting a manuscript for consideration for publication. Manuscripts for publication in AC RESEARCH (4 copies of text and illustrative material) should be submitted to the Editor at the University of North Carolina address. Please include a signed copyright status form; a copy of this document appears on p. 95 of the January 1 issue. Manuscripts for publication in the A-page section should be submitted to the Washington editorial staff. For Individual reprints of AC RESEARCH or A-page articles, please contact the authors directly. Bulk reprints of individual articles are available from ACS. For information, write or call the Distribution office at the ACS Washington address (202-872-4539; fax 202-872-4615). ACS Division of Analytical Chemistry Chair, Joseph L. Glajch (508-671-8413) Secretary, Sarah Rutan (804-367-1298) ACS Information Library Services Education Division Meetings Dept. Member Services Employment Services Public Outreach
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Photon Burst Detection of Single Near-Infrared Fluorescent Molecules Steven A. Soper*, QuincyL. Mattingly, andPradeep Vegunta
740
Effect on Electrothermal Atomization Signals of Contoured Tube Shapes and Isothermality Oscar A. GiiellJamesA. Holcombe*, and Cornelius J. Rademeyer
748
Spectroscopic Separation of Perfluorinated Liquid Mixtures Using Two-Dimensional NMR W. I. Bailey, A. L. Kotz, P. L. McDaniel*, D. M. Parées, F. Κ. Schweighardt, Η. J. Yue *, and C. Anklin Speciation of Iodo Amino Acids by High-Performance Liquid Chromatography with Inductively Coupled Plasma Mass Spectrometric Detection Kikuo Takatera * and Tadashi Watanabe *
752
759
Determination of Methylmercury in Fish Samples Using GC/AA and Sodium Tetraethylborate Derivatization Ralf Fischer, Spyridon Rapsomanikis*', andMeinrat 0. Andreae
763
CS 2 Charge Exchange as a Low-Energy Ionization Technique for Hydrocarbon Characterization Chang S. Hsu * and Kuangnan Qian
767
Differentiation of Aroclors Using Linear Discrimination for Environmental Samples Analyzed by Electron Capture Negative Ion Chemical Ionization Mass Spectrometry Cheng Yu Ma * and Charles K. Bayne
772
Role of Gas Dynamics in Negative Ion Formation in an Atmospheric Sampling Glow Ionization Source David M. Chambers, Scott A. McLuckey, and Gary L. Glish*
778
Investigation of a "Screened" Electrostatic Ion Trap for Analysis of High Mass Molecules by Fourier Transform Mass Spectrometry John A. Castoro, Claus Koster, and Charles L. Wilkins *
784
Preparation of Organic and Water Hydrogen for Stable Isotope Analysis: Effects Due to Reaction Vessels and Zinc Reagent Arndt Schimmelmann * and Michael J. DeNiro
789
Laser Desorption Laser Photoionization Time-of-Flight Mass Spectrometry of Dyes Michael J. Dale, Anita C. Jones, Patrick R. R. Langridge-Smith *, Kevin F. Costello, and Phillip G. Cummins
793
Evaluation of Sequential Extraction for Speciation of Trace Metals in Model Soil Containing Natural Minerals and Humic Acid Shan Xiao-Quan * and Chen Bin
802
A New Approach for the Preparation of a Hydride-Modified Substrate Used as an Intermediate in the Synthesis of Surface-Bonded Materials Chao-Hau Chu, Eltsabetjonsson, Mirva Auvinen, Joseph J. Pesek, and Junior E. Sandoval*
808
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continued on p. 289 A
ANALYTICAL CHEMISTRY, VOL. 65, NO. 6, MARCH 15, 1993 · 287 A
Analytical CHEMISTRY LabGuide The LabGuide is published as the August 15 issue of ANALYTICAL CHEMISTRY. Begun 38 years ago by the JOURNAL, the annual LabGuide edition is designed to be the ultimate buyers' resource for chemists. Its comprehensive coverage includes 2250 categories of laboratory products and services from more than 1700 companies. The 1993 edition features a record 40,000 informative listings detailing manufacturers and distributors of each product and service. Each listing includes the company's phone number for fast action; a more complete listing of the company's address and branch offices is located in a separate section at the back of the book. Sections include Instruments, Equipment, and Supplies (including new subsections on chromatography and spectroscopy); Chemicals and Standards; and Research, Analytical, and Consulting Services. Putting together such a comprehensive and useful guide would be impossible without the suggestions and guidance of our advisory board. Current members include Duane Bartak (University of North Iowa), Bob Hoesly (Mettler Toledo), Paul Preidecker (Gilson), K. C. Warawa (K. C. Associates), Anne Cerino (Anne Cerino Marketing Communications), H. M. Kingston (Duquesne University), Tim Heil (Radian), Susan Olesik (Ohio State University), Rodger Stringham (Merck), Bob Wright (Battelle Pacific Northwest Laboratories), and Sherman Hamel (Parr Instruments).
Instrumentation 1988-1991
in Analytical
Chemistry
This recently published book continues a series begun as Instrumentation in Analytical Chemistry in 1973 by Alan J. Senzel, and continued by Stuart A. Borman in the 1980s as Instrumentation in Analytical Chemistry: Volume 2 and Instrumentation in Analytical Chemistry: 1982-86. Like its predecessors, Instrumentation in Analytical Chemistry 1988-1991 is designed to provide readers with updated overviews of analytical techniques and instrumentation drawn from articles originally published in ANALYTICAL CHEMISTRY'S A pages. The volume begins with an introduction by Royce Murray designed to help readers put into perspective the methodological and instrumental developments that have occurred during the period. The book is divided into six topical areas: Robotics, Computers, and Laboratory Data Management; Atomic and Molecular Spectroscopy; Electroanalytical Chemistry and Chemical Sensors; Separations; Mass Spectrometry; and Surface Analysis. Each section begins with a short introduction designed to provide a context for interpreting the articles that follow and to answer questions such as "What are recent changes in this field?" and "Why are these techniques important?". Copies of Instrumentation in Analytical Chemistry 1988-1991 are available in clothbound ($44.95), paperbound ($28.95), and student ($16.95) editions from the ACS Distribution Office, Dept. 390, 1155 16th St., N.W., Washington, DC 20036 (800-ACS-5558).
Dual Microcolumn Immunoaffinity Liquid Chromatography: An Analytical Application to Human Plasma Proteins Cheryl L. Flurer and Milos Novotny *
817
Horizontal Polymerization of Mixed Trifunctional Silanes on Silica. 2. Application to Chromatographic Silica Gel Mary J. Wirth * and Hafeez O. Fatunmbi
822
Factor Analysis of Phase Transitions and Conformational Changes in Pentaerythritol Tetrasterate Wanjiang Gu *
827
Correspondence Optical Beam Deflection Induced by Enthalpy of a Chemical Reaction and Its Analytical Application Xing-Zheng Wu *, Hiroaki Shindoh, Masaaki Yamada, and Toshiyuki Hobo
834
Location of Double Bonds in Unsaturated Fatty Alcohols by Microderivatization and Liquid Secondary Ion Tandem Mass Spectrometry Takemichi Nakamura *, Tomoko Takazawa, Yasuko Maroyama-Ohki, Hidemi Nagaki, and Takeshi Kinoshita
837
Condensation Nucleation Light Scattering: A New Approach to Development of High-Sensitivity, Universal Detectors for Separations Lori B. Allen and John A. Koropchak *
841
Technical Notes Organic-Phase Enzyme Electrode for the Determination of Trace Water in Nonaqueous Media Joseph Wang* and A. Julio Reviejo
845
Author Index
848
ANALYTICAL CHEMISTRY, VOL. 65, NO. 6, MARCH 15, 1993 · 289 A
