Molecular Spectroscopy Workbench Advances, Applications, and Practical Advice on Modern Spectroscopic Analysis

by Ciurczak, Emil W.

• ISBN13: 9780471180814
• ISBN10: 0471180815
• Edition: 1st
• Format: Hardcover
• Copyright: 1998-03-13
• Publisher: Wiley-Interscience

Summary

The top tools, tips, and techniques of the last decade --at your command. This book compiles and updates the best articles to date from the eleven-year history of Spectroscopy magazine's successful "Molecular Spectroscopy Workbench" column. From the fundamentals of important techniques to novel time- and money-saving ideas, it draws from a broad spectrum of recent developments in the field of molecular spectroscopy, including information on: * Near and midrange infrared techniques * Optical rotation/circular dichroism * UV/Vis and fluorescence * Mass spectrometry * Acousto-optic tunable filters (AOTFs) * Fiber optics * Miscellaneous techniques and new hardware. Articles have been updated where necessary to reflect advances made since their initial publication, and are arranged into sections that cover basic spectroscopic theory, applications, troubleshooting, and product/ conference reviews. Carefully assembled by long-term Spectroscopy columnist Emil Ciurczak, this accessible collection is an excellent practical resource for analytical chemists and others who use spectroscopy in their work.

Author Biography

EMIL W. CIURCZAK has been a columnist for Spectroscopy magazine since 1989. A recognized pioneer in the field of near-infrared spectroscopy for pharmaceutical applications, he is the author of the Handbook of Near-Infrared Analysis.

Table of Contents

Preface	xv	(2)
Acknowledgment	xvii
I. Basic Spectroscopic Theory	1	(42)
I. A. Infrared (Midrange)	1	(12)
1. Echoes of Fundamentals Past or I Don't Think We're Alone in This Spectrum The comparison of fundamental and overtone absorbances in both the mid-IR and the near-IR. SO(2) is used as a model. 6(1), 11(1991)	1	(4)
2. Fourier Transform Spectroscopy: A Dispersive Model Ron Williams discusses interferometry in terms of dispersive processes and models. 6(9), 12(1991)	5	(8)
I. B. Infrared (Near)	13	(8)
1. Near-Infrared Spectroscopy: What it is and What it is Not Some misconceptions about NIR are discussed 4(2), 14(1989)	13	(4)
2. A Closer Look at the Whole Infrared Region A comparison of the hardware and working components of spectrometers used in MIR and NIR is given. 7(3), 12(1992)	17	(4)
I. C. Optical Rotation/Circular Dichroism	21	(22)
1. Chiroptic Phenomena, Part I: Circular Birefringence--Optical Rotation and Optical Rotatory Dispersion Harry G. Brittain discusses the theory behind ORD using math and words to illustrate his points. 6(3), 11(1991)	21	(6)
2. Chioptic Phenomena, Part II: Circular Dichroism Harry G. Brittain demonstrates equipment, theory, and applications of CD in this second part of his article 6(6), 13(1991)	27	(6)
3. Monitoring Conformational Transitions in Synthetic DNA Oligomers Using Circular Dichroism Richard D. Sheardy explains his work with DNA, using the tool of CD to aid in his conformational studies. 6(7), 14(1991)	33	(10)
II. Applied Spectroscopy	43	(272)
II. A. Infrared (Midrange)	43	(36)
1. Near-Infrared Analysis at DuPont: Historical Perspective Eugene S. Taylor talks about the evolution of IR and NIR at DuPont, beginning in 1952. A general historic overview 4(7), 10(1989)	43	(6)
2. Infrared Sample Preparation, or, It's Not the Same Old Grind Various sample presentation techniques are discussed, along with applications and potential problems and solutions. 9(6), 18(1994)	49	(6)
3. Culinary Spectroscopy--FT-IR Analysis of Cooking and Cuisine Gerald J. (Dr. Demento) DeMenna shows that IR does belong in the kitchen. He gives cooking tips and information on the chemistry of food preparation using modern techniques. 4(3), 10(1989)	55	(10)
4. Happiness Is a Warm Sample Photoacoustic spectrometry is discussed, and some examples of its use are given 10(2), 16(1995)	65	(4)
5. Nonstandard Spectroscopic Measurements (or, What To Do When It's Not a Clear Solution or Filter...) Arthur Springsteen gives the low-down on the physics of integrating spheres used in the infrared (and UV/vis/NIR). 12(4), 24(1997)	69	(10)
II. B. Infrared (Near)	79	(86)
1. Part 1: Arterial Analysis with a Novel Near-IR Fiber-Optic Probe. Part 2: Instrument Repair Survey Results Rob Lodder and Lisa Cassis discuss the application of NIR to the determination of LDL and HDL on arterial walls nonintrusively. 5(7), 12(1990)	79	(10)
2. Identification of Actives in Multicomponent Pharmaceutical Dosage Forms Using Near-Infrared Reflectance Analysis Ciurczak and Thomas A. Maldacker use three different algorithms and approaches to identify the active drug and approximate the amount of the same. This work predates principal components analysis and uses early matrix algebra algorithms. A comment by Donald A. Burns follows. 1(1), 36(1986)	89	(10)
3. Evaluation of a Near-Infrared Detector for High-Performance Liquid Chromatography Ciurczak and Frances M. B. Weis discuss the first design and preliminary results of an NIR-HPLC detector. This is the work that became my doctoral thesis. 2(10), 33(1987)	99	(12)
4. Parameters of a Near-IR HPLC Detector, Part I: Limits of Analytical Sensitivity for Reversed-Phase Chromatographic Systems Emil W. Ciurczak and Tracey A. Dickinson discuss the application of NIR to water-based chromatographic systems; quantitation is stressed. 6(2), 12(1991)	111	(8)
5. Parameters of a Near-IR HPLC Detector, Part II: Application to NonAqueous Systems Emil W. Ciurczak, T. Dickinson, and W. R. Murphy discuss non-water-based chromatography from analytical to preparative levels in concentration. Both qualitative and quantitative applications of the detector are discussed. 6(8), 13(1991)	119	(8)
6. The Design Parameters of a Near-Infrared Detector for High-Performance Liquid Chromatography Emil W. Ciurczak and Ina M. Vance discuss the possible mechanical and electronic components for a detector used in absorbance and derivative NIR-HPLC work. 3(9), 56(1988)	127	(8)
7. Determination of Enantiomeric Purity of Valine via Near-Infrared Reflectance Spectroscopy Emil W. Ciurczak, Bruce R. Buchanan, Art Q. Grunke, and David E. Honigs use NIR to determine ratio of D- and I-valine isomers in dry, crystalline racemic mixtures. 3(5), 54(1988)	135	(8)
8. Analysis of Solid and Liquid Dosage Forms Using Near-Infrared Reflectance Spectroscopy Emil W. Ciurczak and Ronald P. Torlini discuss application of NIR to multicomponent solid and liquid dosage forms. 2(3), 41(1987)	143	(8)
9. Determination of Particle Size of Pharmaceutical Raw Materials Using Near-Infrared Reflectance Spectroscopy Emil W. Ciurczak, Ronald P. Torlini, and Michael P. Demkowicz show how diffusely reflected NIR spectra may be used to estimate the mean particle size of the powders tested. 1(7), 36(1986)	151	(8)
10. Applications of Near-IR Spectroscopy in the Pharmaceutical Industry Emil W. Ciurczak and Jim Drennen take a look at the latest NIR research in this important industry. 7(6), 12(1992)	159	(6)
II. C. UV/Vis and Fluorescence	165	(26)
1. Chemometrics: A Powerful Toolbox for UV/vis Spectroscopy Jerry Workman explains, in simple terms, the application of powerful mathematical algorithms to UV/vis. 4(6), 10(1989)	165	(8)
2. A Real "Cool" Technique and Other Musings Low temperature fluorescence hardware and theory is discussed. Divergence of light from dipping fiber optic probes is also discussed as well as potential problems associated with them. 10(7), 18(1995)	173	(4)
3. To Describe in Glowing Terms More fluorescence and phosphorescence applications/theory. 10(3), 14(1995)	177	(4)
4. File Transfer Software for UV/vis Spectroscopy--An OS/2-Based Program for Dynamic Data Exchange John Sanders provides a program suitable for today's and older instruments. 11(6), 24(1996)	181	(10)
II. D. Mass Spectrometry	191	(12)
1. Getting a Charge out of Mass Spectrometry Kenneth Busch describes various methods of ionization in MS. 9(4), 12(1994)	191	(6)
2. Photon Resonance Mass Spectrometry John Wronka describes technique using a tunable IR laser to desorb macromolecules selectively. 5(3), 10(1990)	197	(6)
II. E. Acousto-Optic Tunable Filters	203	(8)
1. A Novel Spectrophotometer System Based on an Acousto-Optical Tunable Filter Theory and operations parameters of a commercial AOTF instrument. Strengths and weaknesses are discussed. 5(1), 10(1990)	203	(4)
2. An AOTF-Illuminated Microscope Work performed by NIH with a Brimrose-manufactured AOTF microscope is described. Wavelengths range from UV to far-IR. 8(2), 12(1993)	207	(4)
II. F. Fiber Optics	211	(10)
1. Shedding Light on Fiber Optics A primer of an article by Scott Wohlstein about the basic theories and some applications of fiber-optic materials. 8(5), 12(1993)	211	(4)
2. Fiber-Optic Multiplexers Bruce Buchanan and Patrick O'Rourke describe the automated fiber-optic multiplexer system developed at Savannah River, GA, for IR and NIR multistation monitoring of some nasty materials 9(3), 12(1994)	215	(6)
II. G. Miscellaneous Techniques/New Hardware	221	(94)
1. What is FT-Raman, and Where Can I Use it? Mary Ann Finch gives a succinct explanation of the theory, hardware, and some applications of FT-Raman 5(6), 12(1990)	221	(12)
2. A Commercial Near-IR Diode-Array Spectrophotometer The theory of diode arrays for NIR as well as two manufacturers' equipment are described herein. 7(9), 12(1992)	233	(4)
3. An LED-Based, Near-IR Process Spectrometer The Katrina, short-wavelength instrument, based on sequentially firing diodes, is described. 8(1), 14(1993)	237	(4)
4. Pictures from Numbers and the Littlest Spectrometer The theory and application of CCDs (charge-coupled devices) are discussed; the Hubble Space Telescope is used as one example, HPLC detectors are examined as spectrometers. 10(1), 14(1995)	241	(4)
5. Hadamard Transform Spectroscopy: Teaching Old Monochromators New Tricks Robert M. Hammaker, William G. Fateley, and David C. Tilotta discuss the first commercial Hadamard instrument. Extensive theory and mathematics are included. [As a further reference, see "Hadamard Transform Infrared Spectroscopy," Z. Zhou and D. C. Tilotta, Spectroscopy, 6(8), 26(1991).] 3(1), 14(1988)	245	(18)
6. Lasers: The Quantum Monkey Wrench Scott Wohlstein discusses the types and parameters of commercially available and experimental lasers. 4(9), 10(1989)	263	(10)
7. Detectors in Infrared Spectroscopy First in the series of four chapters. The various types of detectors for near-, mid-, and far-range infrared instrumentation are described and discussed. Designed as a primer. 8(9), 12(1993)	273	(4)
8. Common Sources and Signal Processing Techniques Used in Vibrational Spectroscopy Second in a series of four chapters. A listing of all potential light sources used in IR/NIR. Designed as a primer. 8(10), 12(1993)	277	(10)
9. Monochromators Used in Vibrational Spectroscopy Third in a series of four chapters. A description of various types of monochromators (dispersive and nondispersive) used in vibrational spectroscopy. Designed as a primer 9(1), 12(1994)	287	(6)
10. Building the Perfect Spectrometer or Pick One from Column A and One from Column B... Last in a series of four related chapters: Tying the previous three chapters (sources, monochromators, and detectors) together in a "how-to" guide for analysts. Designed as a primer. 9(2), 12(1994)	293	(6)
11. Taking the Spectroscopy of Fluids beyond the Limits Valentine J. Rossiter discusses spectroscopy cell used at the extremes of pressure and temperature. 10(6), 18(1995)	299	(8)
12. More Perspectives on the Decade in Spectroscopy Claudio Puebla tells about the updates in software since Spectroscopy first started publishing in "Ten Years of Computational Chemistry." Near-field scanning optical microscopy is discussed by Dan Higgins. In "Once again into the Fray," Ciurczak discusses how to select the number of samples for calibration of an on-line instrument. 11(1), 24(1996)	307	(8)
III. General Troubleshooting	315	(42)
1. Purgamenta Iniunt, Purgamenta Exiunt A look at the folly of trying to correct poor spectra with the power of computers. Caveat emptor is the key. (A "Latin" flavor!). 7(1), 12(1992)	315	(4)
2. A Look at Validation for Spectroscopic Instrumentation: The FDA Has Taken the Lead The concepts behind the need and procedures used in validation. The definition of "validation" is examined. 8(7), 12(1993)	319	(6)
3. Chemical Intuition in Analytical Testing: A Case Study Elisa Lyth and Lily M. Ng show how a little forensics thinking in everyday lab work helped solve a problem. An unknown peak led to an understanding of a problem. 9(5), 12(1994)	325	(6)
4. Two Valuable Tools for Instrument Evaluation: JCAMP.DX and Price Tags A new standard file structure, similar to ASCII and the cost/value relationship of new instruments are discussed. 4(8), 12(1989)	331	(4)
5. Nobody Knows the Troubles I've Seen... Several instrumentation problems solved. Moisture on IR windows, alcohol used to stabilize alkenes and alkynes. 9(8), 22(1994)	335	(4)
6. Some More Uh-Ohs for the Vibrational Spectroscopist Assorted troubleshooting tips: dying lamps, stray light, fiberoptics, diagnostics for mulls, thin films, and KBr pellets. 9(9), 28(1994)	339	(4)
7. Learning Tools: Chemistry Education and Molecular Modeling The curricula in secondary schools as well as college and graduate teaching methodology are discussed. Molecular modeling as a tool is looked at along with several programs available. 8(3), 12(1993)	343	(6)
8. What's in a Name? And Reflections on a Dusty Surface More troubleshooting tips on cleaning cuvettes, etc. 9(7), 16(1994)	349	(4)
9. Questions and Answers on Process Analysis: Tips for Selecting and Calibrating IR Instruments Some questions arising from the ACS Short Course on NIR, but applied to IR as well. 10(9), 18(1995)	353	(4)
IV. Review Columns	357
IV. A. Conferences	357	(24)
1. A Review of the Third International Conference on Near-Infrared Spectroscopy Program highlights and details on nonagricultural papers presented in Brussels in June, 1990. 5(8), 14(1990)	357	(4)
2. "What's New in Spectroscopy?" A Report on PittCon '92 in New Orleans Notable UV/vis/near-IR papers given at PittCon 1992. 7(4), 16(1992)	361	(2)
3. A Report from the Sixth International Diffuse Reflectance Conference A review of the technical program from Chambersburg, PA, on the 1992 biennial conference. 7(8), 12(1992)	363	(4)
4. "What's New in Spectroscopy?" PittCon '93 in Atlanta Scope of discussion and important papers presented at the annual conference in 1993. 8(4), 16(1993)	367	(2)
5. Near-Infrared Topics from the 1994 PittCon Important topics discussed in 1994. 9(4), 29(1994)	369	(2)
6. Near-Infrared Topics from the 1995 PittCon Important topics discussed in 1995. 10(5), 42(1995)	371	(2)
7. The Good Old Days, or What? Musings on the last 10 years for the anniversary issue. 10(8), 22(1995)	373	(4)
8. Review of the 8th International Diffuse Reflectance Conference (1996): or "Round Up the Usual Suspects!" The Chambersburg meeting is reviewed for content and impact. 12(2), 15(1997)	377	(4)
IV. B. New Equipment and Miscellaneous	381
1. A New Beginning and a Wrapup of What's New in Instrumentation A review of new instruments since PittCon 1988 and the first column written by Ciurczak. 4(1), 18(1989)	381	(8)
2. Pittsburgh Conference Review: 1989 in Atlanta A review of spectroscopic hardware, software, and accessories at the Pittsburgh Conference. 4(4), 10(1989)	389	(20)
3. Instrument Service Survey A call to users for instrument maintenance info. 5(2), 12(1990)	409	(4)
4. 1990 PittCon Product Wrapup, Part 1: Instrumentation for Molecular Spectroscopy Instruments, software, and accessories for spectroscopic work, listed by increasing wavelength. 5(4), 12(1990)	413	(20)
5. "What's New in Spectroscopy Instrumentation?" 1991 PittCon Wrapup Last review done on ALL equipment from UV-vis through far-IR, MS, NMR, etc. 6(4), 12(1991)	433	(18)
6. Internet Sites for Infrared and Near-Infrared Spectrometry, Part I: Online Instruction and Direct Communication Rob Lodder and Elizabeth G. Kraemer present a list of Web sites and newsgroups for the IR community as well as some commentary of the future impact of electronic media on scientific education and publishing. 11(7), 24(1996)	451	(10)
7. Internet Sites for Infrared and Near-Infrared Spectrometry, Part II: Promotional Sites and Online Publications The second part of the listing of Web sites compiled by Rob Lodder and Elizabeth G. Kraemer, focusing on promotional sites and online publications. 11(8), 17(1996)