Analytical Spectroscopy

Total Page:16

File Type:pdf, Size:1020Kb

Analytical Spectroscopy ANAL YTICAL CHEMISTRY SYMPOSIA SERIES - volume 19 analytical spectroscopy Proceedings of the 26th Conference on Analytical Chemistry in Energy Technology, KnoxviUe, TN, October 11-13, 1983 CONF-831025- edited by DESS 014573 W.S. Lyon An&lytical Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, TN, U.S.A. Sponsored by the Analytical Chemistry Division, Oak Ridge National Laboratory, operated by Union Carbide Corporation for the Department of Energy under Contract No. W-7405*ng-26. DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsi- bility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Refer- ence herein io any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recom- mendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. ELSEVIER Amsterdam - Oxford - New York - Tokyo 1984 ELSEVIER SCIENCE PUBLISHERS B.V. Molenwerf 1 P.O. Box 211,1000 AE Amsterdam, The Netherlands Distributon for the United States and Canada: ELSEVIER SCIENCE PUBLISHING COMPANY INC. 52, Vanderbilt Avenue New York, NY 10017, U.S.A. The Government reserves for itself and others acting on its behalf a royalty free, nonexclusive, irrevocable, world-wide license for governmental purposes to publish, distribute, translate, duplicate, exhibit, and perform any such data copy- righted by the contractor. Library of Congress Cataloging in Publication Data Conference on Analytical Chemistry in Energy Technology (^oth : Uoi : Kno:<v:lle, Tenn.) Analytical siiectro^copy. (Analytic^1 eheir.istry symposia series ; v. 19) Include;: indOK. 1. Spectrum analysis—Congresses. I. Lyon, VI. S. (Millions.) II. Title. III. Series. QD9;.Ct,33 I9b3 5li3'.085S - SU-3975 ISBN Q-hhk-h?312-5 ISBN 0-444-42312-5 (Vol. 191 ISBN 0-444-41786-9 (Series) © Elsevier Science Publishers B.V.. 1984 All rights reserved. No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, mechanical, photocopying, recording or other- wise, without the prior written permission of the publisher, Elsevier Science Publishers B.V., P.O. Box 330,1000 AH Amsterdam, The Netherlands Printed in The Netherlands CONTENTS Analytical Chemistry Symposia Series XI Preface XIII Conference Commi ttee .... „ XIV LASERS Recent Applications of Lasers in Analytical Chemistry, F.E. Lytle 3 Determination of Uranium in Plutonium Solutions by User Induced Fluorescence, <7.E. Xoung, P'T. Deaaon , 7 Instrumentation for Remote Sensing Over Fiber Optics, T. Hiveehfeld, G. Haugen, F. Milanoviah > 13 Fiber Optics Temperature and Pressure Probe, T, Hirsahfeld, F. Vang, G. Haugen, G. Hieftje 19 On-Line Uranium Determination Using Remote Fiber Fiuorimetry, R.A. Maistvom, T. Hireahfeld 25 Versatility of Laser Induced Fluorescence Line Narrowing in Chemicjl Analysis, M.J- McGlade, J.M. Hayes, G.J. Small, V. Heisig, A .M. Jeffrey , 31 Matrix-Isolation Photoacoustic Spectroscopy, R.W. Shaa, h'.E. Howell G. Mamankov, E.L. Wehry 37 Selective Fluorometric Determinations by Laser-Induced Matrix Isolation Fluorescence Spectrometry, E.L. Wehry 43 Metal Surface Enhanced Fluorescence, T.D, Harris, A.M. Glass, D.H. Olson 49 Prospects for Single-Molecule Detection in Liquids by Laser-Induced Fluorescence, Af. Trkula, N.J. Doviahi, J.C. Martin, J.H. Jett, R.A. Keller 53 Kinetic Analysis of Laser Induced Phosphorescence in Uranyl Phosphate for Improved Analytical Measurements, S.A. Bushaa 57 VI Performance Appraisal Studies of Laser-Enhanced Ionization in Flames -- The Determination of Nickel in Petroleum Products, G*C-. Turk, G.J. Havrilla, J.D. Webb, A.R. Fovetev 63 Laser Spectroscopic Studies of Solvation Phenomena, 14.J. Wirth 69 Laser Spectroscopic Studies of Vibrational Overtones. Influence of Molecular Conformation on Overtone Energies, H.L. Fang, R.L. Stafford 75 Infrared Laser Spectroscopy Using a Long Pathlength Absorption Cell, K.C. Kim, R.A. Srieemeieter 81 MASS SPECTROMETRY Some Advances in Inorganic Analytical Mass Spectrometry, H.J. Svea 89 A State-of-the-Art Mass Spectrometer System for Determination of Uranium and Plutonium Isotopic Distributions in Process Samples, C.A. Poison .. 103 Americium Determination Using an Isotope Dilution Mass Spectrometry Technique, D. V. Crawford, R. D. Peavy , m An In-Line Analyzer for Monitoring Gas Composition in Tritium Purification Processes - Design, P. Chastagnev 119 Application of Mass Spectrometry to Fuels and Materials Testing at FFTF, C.E. Plucineki, M.U. Gokeen, J.J. McCom 127 Improved Precision and Speed of Thermal lonisation Mass Spectrometry With a Mul ticollector, P.J. Turner, J.E. Canble, R.C. Hainee ,. 123 Resonance Ionization Mass Spectrometry of Iron—Quantitative Aspects, J.D. Fassett, L.J. Moore, J.C. Travis , 137 Isotopic Measurements of Uranium and Plutonium by Resonance Ionization Mass Spectrometry, D.£. Donahue, J.P. Young, D.H. Smith 143 Sputter Initiated Resonance Ionization Spectroscopy for Trace Element Analysis, J.E. Rirke, H.W. Sekmitt, G.S. Hurst, W.M. Faiybank, Jr 149 Vll Resonance Ionization Mass Spectrometry at Los Alamos National Laboratory, N.S. Jlogar, S.V. Downey, ft.A. Keller, CM. Miller 155 The Determination of Uranium in Urine by Isotope Dilution Mass Spectrometry Using Resin Bead Loading, M.P. Nay, R.L. Walker, T.G. Scott, F.F. Dyer, J.R. Stokely 161 SIMS Study of Compositional Changes Observed in a PuO2 Heat Source Cladding Alloy, U.H. Christie, D.H. Taylor, R.E. Eby, D. PaVone 167 Laser Enhanced Ionization in Glow Discharge Mass Spectrometry, V.V. Harrison, P.J. Savickas, R.K, Wxreua, K.fl. Heae 173 Examination of Excited State Populations in Sputtering Using Multiphoton Resonance lonization, F.M. Kimook, J.P. Baxter, D.L. Pappas, F.ff. Kobrin, It. Hnogmd 179 PLASMA A Preliminary Study on the Determination of Boron and Cadmium Impurities in Uranium Oxide and Uranium Metals by Inductively Coupled Plasma- Atomic Emission Spectroscopy, B.R. Bear, M.C. Edelson, B. Gopalan, V.A. Faeeel 1*7 Analyses of Nuclear Fuel and High-Level Waste by Inductively Coupled Plasma-Emission Soectroscopy, C.J. Coleman 195 Determination of Trace Impurities in Uranium Matrices by Inductively Coupled Plasma-Atomic Emission Spectrometry, A.A. Haloum, R.B. Farrav, E.A. Hester, R.V. Morrou 201 Measurement of Rhodium and Palladium in Selected Hanford Defense Wastes, U.H. West, C.S. Homi, C. H. Hunter 203 Considerations for the Installation of an Inductively Coupled Plasma for the Analysis of Radioactive Samples, C.T. Apel, D.L. Gallimore 213 Evolution of Containment Facilities for Spectroscopic Analysis at Rockwell Hanford Operations, J.M. Hiller 219 VIII A New Facility for High Resolution Inductively Coupled Plasma-Atomic Multielement Emission Spectroscopy of Radioactive Materials, M.C. Edeleon, V.A. Faesel 227 Plans for Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) Analysis of Impurities in Plutonium Materials at Rocky Flats, C.E. Michel, G.E. Bvoun 235 NUCLEAR Utilization of the Intense Pulsed Neutron Source (IPNS) at Argonne National Laboratory for Neutron Activation Analysis, R.R. HainHoh, l.R. Greenwood, R.J. Popek, A.W. Sahulke, Jr. 243 Heavy-Ion Induced X-Ray Satellite Emission as a Chemical Probe, T.M. Roeseel, J.M. Dale, l.D. Hulett, H.F. Kvauee, S. Raman, C.R. Vane, J.P. Young 249 Analytical Measurements of Actinide Migration in a Laboratory-Simulated Basalt HLW Repository, D.L. Bothers, T.J. Gerding, S.M. Fried, G.F. Vandegrift, M.G, Seitz 255 Analytical Research at the Institute of Radiochemistry, Nuclear Research Center, Karlsruhe, FRG, B. Gantnev, E. Mairka, H. Ruf, H.J. Aohe 263 Comparison of Burnup Methods for (Th.U)Og Fuel, L.U. Green, R.H. Caesidy, W.J. Edaarde, C.H. Knight 273 Irradiation and Gamma-Ray Spectrometric Parameters for 1Z9I Neutron Activation Analysis, J.H. Kaye, R.S. Strebin, Jr., F.P. Brauer, U.A. Mitzlaff 279 Monitoring of Radionucl1des and Metallic Impurities in the KNK-II Primary Sodium, H.H. Sham, K.Ch. Stade 285 Surface Characterization of Leadscrews Taken from the TMI-2 Reactor Vessel, K.J. Hofetetter, H. Soaeneekuse, V.F. Bast on 293 An n-Type High Purity Germanium Detector-Based On-Line Rapid Coal Analysis System, F.B. leVert, W.W. Managcm 299 IX Automated Gamma Spectrometry and Data Analysts on Radiometric Neutron Dosimeters, tf.r. mtevmoto 309 Environmental Applications for an Intrinsic Germanium Well Detector, P. Stegnxr, J.S. Eldridge, N.A. Teasley, T.W. Cakes 313 OTHER SPECTROSCOPIC TECHNIQUES Sampling and Characterization of Aerosols Formed In the Atmospheric Hydrolysis of UF6, V.D. Bostiok, W.H. MoCulla, P.W. Piekrell, D.A. Branm 321 Applications of Laser Spectroscopy for Species Determination 1n Fission Product Release Experiments, W.H. HaCuXla, G.E. Nelson, R.A. horena ... 327 Spectroscopic Diagnostics of an Argon Plasma Jet Seeded with Uranium, O.K. Anderson 333 General-Purpose Chemical Analyzer for Online Analyses of Radioactive Solutions, W.A. Spencer, J.W. Kronberg 337 Influence of Uranyl 01butyl phosphate on the UV/VIS Spectrophotometric Online Monitoring of Uranium In Tributylphosphate/Hydrocarbon Solvent, E.T. Creech, A.C. Butenberg, R.W. Smtihwick.* R.D. Seals 343 Controlled-Potential-Coulometric Determination of Uranium at a Platinum Electrode, V.M. Saponara, D.D. Jackson 345 Atomic Absorption Spectrophotometric Methods for the Determination of Phosphorous and Silicon in Steel, J.P. McCarthy, B.B. Vwm, c. Kinard 349 Analysis of Molecular Hydrogen Using Spontaneous Raman Spectroscopy, K.
Recommended publications
  • Chapter 9 Titrimetric Methods 413
    Chapter 9 Titrimetric Methods Chapter Overview Section 9A Overview of Titrimetry Section 9B Acid–Base Titrations Section 9C Complexation Titrations Section 9D Redox Titrations Section 9E Precipitation Titrations Section 9F Key Terms Section 9G Chapter Summary Section 9H Problems Section 9I Solutions to Practice Exercises Titrimetry, in which volume serves as the analytical signal, made its first appearance as an analytical method in the early eighteenth century. Titrimetric methods were not well received by the analytical chemists of that era because they could not duplicate the accuracy and precision of a gravimetric analysis. Not surprisingly, few standard texts from the 1700s and 1800s include titrimetric methods of analysis. Precipitation gravimetry developed as an analytical method without a general theory of precipitation. An empirical relationship between a precipitate’s mass and the mass of analyte— what analytical chemists call a gravimetric factor—was determined experimentally by taking a known mass of analyte through the procedure. Today, we recognize this as an early example of an external standardization. Gravimetric factors were not calculated using the stoichiometry of a precipitation reaction because chemical formulas and atomic weights were not yet available! Unlike gravimetry, the development and acceptance of titrimetry required a deeper understanding of stoichiometry, of thermodynamics, and of chemical equilibria. By the 1900s, the accuracy and precision of titrimetric methods were comparable to that of gravimetric methods, establishing titrimetry as an accepted analytical technique. 411 412 Analytical Chemistry 2.0 9A Overview of Titrimetry We are deliberately avoiding the term In titrimetry we add a reagent, called the titrant, to a solution contain- analyte at this point in our introduction ing another reagent, called the titrand, and allow them to react.
    [Show full text]
  • Analytical Chemistry Laboratory Manual 2
    ANALYTICAL CHEMISTRY LABORATORY MANUAL 2 Ankara University Faculty of Pharmacy Department of Analytical Chemistry Analytical Chemistry Practices Contents INTRODUCTION TO QUANTITATIVE ANALYSIS ......................................................................... 2 VOLUMETRIC ANALYSIS .............................................................................................................. 2 Volumetric Analysis Calculations ................................................................................................... 3 Dilution Factor ................................................................................................................................ 4 Standard Solutions ........................................................................................................................... 5 Primary standard .............................................................................................................................. 5 Characteristics of Quantitative Reaction ......................................................................................... 5 Preparation of 1 L 0.1 M HCl Solution ........................................................................................... 6 Preparation of 1 L 0.1 M NaOH Solution ....................................................................................... 6 NEUTRALIZATION TITRATIONS ...................................................................................................... 7 STANDARDIZATION OF 0.1 N NaOH SOLUTION ......................................................................
    [Show full text]
  • Analytical Chemistry in the 21St Century: Challenges, Solutions, and Future Perspectives of Complex Matrices Quantitative Analyses in Biological/Clinical Field
    Review Analytical Chemistry in the 21st Century: Challenges, Solutions, and Future Perspectives of Complex Matrices Quantitative Analyses in Biological/Clinical Field 1, 2, 2, 3 Giuseppe Maria Merone y, Angela Tartaglia y, Marcello Locatelli * , Cristian D’Ovidio , Enrica Rosato 3, Ugo de Grazia 4 , Francesco Santavenere 5, Sandra Rossi 5 and Fabio Savini 5 1 Department of Neuroscience, Imaging and Clinical Sciences, University of Chieti–Pescara “G. d’Annunzio”, Via dei Vestini 31, 66100 Chieti, Italy; [email protected] 2 Department of Pharmacy, University of Chieti-Pescara “G. d’Annunzio”, Via Dei Vestini 31, 66100 Chieti (CH), Italy; [email protected] 3 Section of Legal Medicine, Department of Medicine and Aging Sciences, University of Chieti–Pescara “G. d’Annunzio”, 66100 Chieti, Italy; [email protected] (C.D.); [email protected] (E.R.) 4 Laboratory of Neurological Biochemistry and Neuropharmacology, Fondazione IRCCS Istituto Neurologico Carlo Besta, Via Celoria 11, 20133 Milano, Italy; [email protected] 5 Pharmatoxicology Laboratory—Hospital “Santo Spirito”, Via Fonte Romana 8, 65124 Pescara, Italy; [email protected] (F.S.); [email protected] (S.R.); [email protected] (F.S.) * Correspondence: [email protected]; Tel.: +39-0871-3554590; Fax: +39-0871-3554911 These authors contributed equally to the work. y Received: 16 September 2020; Accepted: 16 October 2020; Published: 30 October 2020 Abstract: Nowadays, the challenges in analytical chemistry, and mostly in quantitative analysis, include the development and validation of new materials, strategies and procedures to meet the growing need for rapid, sensitive, selective and green methods.
    [Show full text]
  • "Thermal Analysis and Calorimetry," In
    Article No : b06_001 Thermal Analysis and Calorimetry STEPHEN B. WARRINGTON, Formerly Anasys, IPTME, Loughborough University, Loughborough, United Kingdom Gu€NTHER W. H. Ho€HNE, Formerly Polymer Technology (SKT), Eindhoven University of Technology, Eindhoven, The Netherlands 1. Thermal Analysis.................. 415 2.2. Methods of Calorimetry............. 424 1.1. General Introduction ............... 415 2.2.1. Compensation of the Thermal Effects.... 425 1.1.1. Definitions . ...................... 415 2.2.2. Measurement of a Temperature Difference 425 1.1.2. Sources of Information . ............. 416 2.2.3. Temperature Modulation ............. 426 1.2. Thermogravimetry................. 416 2.3. Calorimeters ..................... 427 1.2.1. Introduction ...................... 416 2.3.1. Static Calorimeters ................. 427 1.2.2. Instrumentation . .................. 416 2.3.1.1. Isothermal Calorimeters . ............. 427 1.2.3. Factors Affecting a TG Curve ......... 417 2.3.1.2. Isoperibolic Calorimeters ............. 428 1.2.4. Applications ...................... 417 2.3.1.3. Adiabatic Calorimeters . ............. 430 1.3. Differential Thermal Analysis and 2.3.2. Scanning Calorimeters . ............. 430 Differential Scanning Calorimetry..... 418 2.3.2.1. Differential-Temperature Scanning 1.3.1. Introduction ...................... 418 Calorimeters ...................... 431 2.3.2.2. Power-Compensated Scanning Calorimeters 432 1.3.2. Instrumentation . .................. 419 2.3.2.3. Temperature-Modulated 1.3.3. Applications ...................... 419 Scanning Calorimeters . ............. 432 1.3.4. Modulated-Temperature DSC (MT-DSC) . 421 2.3.3. Chip-Calorimeters .................. 433 1.4. Simultaneous Techniques............ 421 2.4. Applications of Calorimetry.......... 433 1.4.1. Introduction ...................... 421 2.4.1. Determination of Thermodynamic Functions 433 1.4.2. Applications ...................... 421 2.4.2. Determination of Heats of Mixing . .... 434 1.5. Evolved Gas Analysis..............
    [Show full text]
  • Chromatography Programme Course 6 Credits Analytisk Kemi - Kromatografi NKEB10 Valid From: 2018 Spring Semester
    1(9) Analytical Chemistry - Chromatography Programme course 6 credits Analytisk kemi - Kromatografi NKEB10 Valid from: 2018 Spring semester Determined by Board of Studies for Chemistry, Biology and Biotechnology Date determined LINKÖPING UNIVERSITY FACULTY OF SCIENCE AND ENGINEERING LINKÖPING UNIVERSITY ANALYTICAL CHEMISTRY - CHROMATOGRAPHY FACULTY OF SCIENCE AND ENGINEERING 2(9) Main field of study Chemical Engineering, Chemistry Course level First cycle Advancement level G1X Course offered for Chemical Analysis Engineering, B Sc in Engineering Chemistry, Bachelor´s Programme Biology Chemical Biology, Bachelor's Programme Entry requirements Note: Admission requirements for non-programme students usually also include admission requirements for the programme and threshold requirements for progression within the programme, or corresponding. Prerequisites General Chemistry, Organic Chemistry, Calculation tools for chemistry students, Analytical Chemistry Intended learning outcomes The aim of the course is to give fundamental theoretical, practical and instrumental knowledge in the field of analytical separation techniques. After completing this course the student should be able to: Give an account of basic concepts within the area of analytical separation techniques (chromatography and capillary electrophoresis). Describe the principles and construction of instruments used for chromatography LINKÖPING UNIVERSITY ANALYTICAL CHEMISTRY - CHROMATOGRAPHY FACULTY OF SCIENCE AND ENGINEERING 3(9) and capillary electrophoresis. Explain the chemical principles of analytical separation methods. Qualitatively and quantitatively evaluate data obtained from chromatographic and electrophoretic separations. Course content Theory of chromatographic separation. Gas chromatography (GC) including sample injection, separation and detection. High performance liquid chromatographic (HPLC) methods such as normal phase and reversed phase HPLC, ion chromatography and size- exclusion chromatography. Theory and principles of capillary electrophoresis. Mass spectrometry.
    [Show full text]
  • Electrochemical Methods of Analysis. Basic Elec
    JS CH3403 Interdisciplinary Chemistry Module 1. 2013/2014. Analytical Chemistry: Electrochemical methods of analysis. Basic Electroanalytical Chemistry. Potentiometric,Voltammetric and Coulometric measurement techniques. Professor Mike Lyons School of Chemistry TCD Room 3.2 Main Chemistry Building [email protected] Electro-analytical Chemistry. Electroanalytical techniques are concerned with the interplay between electricity & chemistry, namely the Electro-analytical chemists at work ! measurement of electrical quantities Beer sampling. such as current, potential or charge Sao Paulo Brazil 2004. and their relationship to chemical parameters such as concentration. The use of electrical measurements for analytical purposes has found large range of applications including environmental monitoring, industrial quality control & biomedical analysis. EU-LA Project MEDIS : Materials Engineering For the design of Intelligent Sensors. Outline of Lectures • Introduction to electroanalytical chemistry: basic ideas • Potentiometric methods of analysis • Amperometric methods of analysis • Coulombic methods of analysis J. Wang, Analytical Electrochemistry, 3rd edition. Wiley, 2006 R.G. Compton, C.E. Banks, Understanding Voltammetry, 2nd edition, Imperial College Press,2011. C.M.A. Brett, A.M.Oliveira Brett, Electrochemistry: Principles, methods and applications, Oxford Science Publications, 2000. Why Electroanalytical Chemistry ? Electroanalytical methods have certain advantages over other analytical methods. Electrochemical analysis allows for the determination
    [Show full text]
  • Chapter 7 High-Performance Liquid Chromatography (HPLC)
    NEPHAR 201 Analytical Chemistry II Chapter 7 High-Performance Liquid Chromatography (HPLC) Assist. Prof. Dr. Usama ALSHANA 1 Week Topic Reference Material Instructor 1 Introduction Instructor’s lecture notes Alshana [14/09] Principles of Instrumental Analysis, Chapter 6, 2 An introduction to spectrometric pages 116-142 Alshana [21/09] methods Enstrümantal Analiz- Bölüm 6, sayfa 132-163 Principles of Instrumental Analysis, Chapter 7, 3 Components of optical pages 143-191 Alshana [28/09] instruments Enstrümantal Analiz- Bölüm 7, sayfa 164-214 Principles of Instrumental Analysis, Chapter 9, 4 Atomic absorption and emission pages 206-229, Chapter 10, pages 230-252 Alshana [05/10] spectrometry Enstrümantal Analiz- Bölüm 9, sayfa 230-253, Bölüm 10 sayfa 254-280 Principles of Instrumental Analysis, Chapter 13, 5 Ultraviolet/Visible molecular pages 300-328 Alshana [12/10] absorption spectrometry Enstrümantal Analiz- Bölüm 13, sayfa 336-366 Principles of Instrumental Analysis, Chapter 16, 6 Omitted Infrared spectrometry pages 380-403 Alshana [19/10] Enstrümantal Analiz- Bölüm 16, sayfa 430-454 Quiz 1 (12.5 %) 7 Principles of Instrumental Analysis, Chapter 26, Alshana [26/10] Chromatographic separations pages 674-700 Enstrümantal Analiz- Bölüm 26, sayfa 762-787 8 [02- MIDTERM EXAM (25 %) 07/11] 9 High-performance liquid Principles of Instrumental Analysis, Chapter 28, Alshana [09/11] chromatography (1) pages 725-767 10 High-performance liquid Enstrümantal Analiz- Bölüm 28, sayfa 816-855 Alshana [16/11] chromatography (2) Principles
    [Show full text]
  • An Introduction to Instrumental Methods of Analysis
    An Introduction to Instrumental Methods of Analysis Instrumental methods of chemical analysis have become the principal means of obtaining information in diverse areas of science and technology. The speed, high sensitivity, low limits of detection, simultaneous detection capabilities, and automated operation of modern instruments, when compared to classical methods of analysis, have created this predominance. Professionals in all sciences base important decisions, solve problems, and advance their fields using instrumental measurements. As a consequence, all scientists are obligated to have a fundamental understanding of instruments and their applications in order to confidently and accurately address their needs. A modern, well-educated scientist is one who is capable of solving problems with an analytical approach and who can apply modern instrumentation to problems.1 With this knowledge, the scientist can develop analytical methods to solve problems and obtain appropriately precise, accurate and valid information. This text will present; 1) the fundamental principles of instrumental measurements, 2) applications of these principles to specific types of chemical measurements (types of samples analyzed, figures of merit, strengths and limitations), 3) examples of modern instrumentation, and 4) the use of instruments to solve real analytical problems. The text does not include information on every possible analytical technique, but instead contains the information necessary to develop a solid, fundamental understanding for a student in an upper level undergraduate class in instrumental analysis. 1-1. Background Terminology: Before presenting the complete picture of a chemical analysis, it is important to distinguish the difference between an analytical technique and an analytical method.2 An 1 analytical technique is considered to be a fundamental scientific phenomenon that has been found to be useful to provide information about the composition of a substance.
    [Show full text]
  • Electrochemistry a Chem1 Supplement Text Stephen K
    Electrochemistry a Chem1 Supplement Text Stephen K. Lower Simon Fraser University Contents 1 Chemistry and electricity 2 Electroneutrality .............................. 3 Potential dierences at interfaces ..................... 4 2 Electrochemical cells 5 Transport of charge within the cell .................... 7 Cell description conventions ........................ 8 Electrodes and electrode reactions .................... 8 3 Standard half-cell potentials 10 Reference electrodes ............................ 12 Prediction of cell potentials ........................ 13 Cell potentials and the electromotive series ............... 14 Cell potentials and free energy ...................... 15 The fall of the electron ........................... 17 Latimer diagrams .............................. 20 4 The Nernst equation 21 Concentration cells ............................. 23 Analytical applications of the Nernst equation .............. 23 Determination of solubility products ................ 23 Potentiometric titrations ....................... 24 Measurement of pH .......................... 24 Membrane potentials ............................ 26 5 Batteries and fuel cells 29 The fuel cell ................................. 29 1 CHEMISTRY AND ELECTRICITY 2 6 Electrochemical Corrosion 31 Control of corrosion ............................ 34 7 Electrolytic cells 34 Electrolysis involving water ........................ 35 Faraday’s laws of electrolysis ....................... 36 Industrial electrolytic processes ...................... 37 The chloralkali
    [Show full text]
  • Analytical Chemistry Chemical Analysis
    Analytical chemistry Chemical analysis a) Qualitative b) Quantitative analysis analysis Qualitative analysis Definition : Knowing the of substance present in the solution.( i.e. it’s quality). Examples : ( Iron (Fe), Copper (Cu), Calcium, ………etc.) Identification of chemical components is done by: 1) Physically : (Color, Odor, Shape) 2) Chemically : (Components of the sample) Quantitative analysis Definition: Knowing quantity of substance present in the solution. Examples : the quantity of a certain substance in the sample solution (10% Fe, 3% Na, 5% Cl, ………………etc.). 1) Traditional method: Volumetric analysis: Knowing the concentration of the sample, example: (titration method). 2) Modern method: Instrumental technique: (Spectrophotometric analysis) Important Definitions Atom Atom • It’s the smallest building unit for an element. • It consists of a nucleus containing combination of neutrons and protons. • The number of protons determines the identity of the element. • One of more electrons bound to the nucleus by electrical attraction. • Examples : Carbon ( C), Hydrogen ( H), Oxygen ( O), Nitrogen( N), Iron ( Fe ), Sulfur ( S), Aluminum ( Al ), ……….etc. Atom Atomic weight (At.wt) • Its the weight of a single atom. • Its the summation of number of protons and neutrons . • It’s unit atomic mass unit (a.m.u.) • It’s written under elements in the periodic table • Examples: 1. At.wt of Hydrogen (H) = 1 a.m.u. 2. At.wt of Carbon (C) = 12 a.m.u. 3. At.wt of Oxygen (O) = 16 a.m.u. 4. At.wt of sodium (Na ) = 23 a.m.u. 5. At.wt of Chloride (Cl ) = 35.5 a.m.u. Molecule Molecule • It consists of 2 or more atoms which have chemically combined to form a single species.
    [Show full text]
  • High Performance Liquid Chromatography Method Development and Chemometric Analysis of Ecstasy and Cocaine
    institlüld ictterkcnny TeicneoUiochti institute lyit (.«Ulf C*»n«lon of Technology High performance liquid chromatography method development and chemometric analysis of ecstasy and cocaine Kim McFadden Supervisors Dr. B. F. Carney, Letterkenny Institute of Technology Dr. D. O'Driscoll, Forensic Science Laboratory, Dublin Submitted to Higher bducation and Training Awards Council (HETAC) in fulfilment for the requirements for the degree of Doctor of Philosophy HPLC method development & chemomelric analysis of ecstasy & cocaine Declaration I hereby declare that the work herein, submitted for Ph.D. in Analytical Science at Letterkenny Institute of Technology, is the result of my own investigation, except where reference is made to published literature. I also certify that the material submitted in this thesis has not been previously submitted for any other qualification. Kim McFadden 1 HPLC method development & chemometric analysis of ecstasy & cocaine Table of Contents Declaration 1 Abstract 5 List of Abbreviations 7 List of Figures 10 List of Tables 14 List of Presentations and Publications 16 Acknowledgments 18 Chapter 1: Literature review. 19 1.1. Introduction. 20 1.2. Drugs of abuse. 21 1.2.1. Narcotics. 22 1.2.2. Depressants. 24 1.2.3. Stimulants. 24 1.2.4. Hallucinogens. 25 1.2.5. Ecstasy. 26 1.2.6. Cocaine. 31 1.3. Current analytical techniques for forensic drug analysis. 34 1.3.1. Spectrometric methods. 34 1.3.2. Chromatographic methods. 36 1.4. Fundamentals of High Performance Liquid Chromatography. 40 1.4.1. Chromatographic interactions. 40 1.4.2. Mobile phase. 41 1.4.3. The column. 42 1.4.4.
    [Show full text]
  • Analytical Chemistry
    ANALYTICAL CHEMISTRY - INFRARED SPECTROSCOPY Commonly referred to as IR spectroscopy, this technique allows chemists to identify characteristic groups of atoms (functional groups) present in molecules. C H C H C C THE FINGERPRINT REGION - 1500CM-1 TO 500CM-1 Stretch Stretch Stretch The fingerprint region of the spectrum contains a complex set of absorptions, which are unique to each compound. Though these are M M M hard to interpret visually, by comparison with references they allow identification of specific compounds. ALKENE ALDEHYDE ALKENE AROMATICS C H C H C C C O C C C O C X Stretch Stretch Stretch Stretch Stretch Stretch Stretch N S M W S M S M ALKYNE ALKANE ALKYNE CARBONYLS AROMATICS ESTERS, ETHERS, ALCOHOLS, ALKYL CHLORIDE (850-550) CARBOXYLIC ACIDS ALKYL BROMIDE (690-515) ACID N H C N N H C H C H C H C H Stretch Stretch ANHYDRIDE Bend Bend, Rock Wag Bend Bend M V M M M S S B ACYL CHLORIDE 1˚& 2˚AMINE NITRILE 1˚AMINE ALKANE HALOALKANE ALKENE ALKENE AMIDE ESTER O H O H N O N O C N O H N H Stretch Stretch AMIDE Asymm. Stretch Symm. Stretch Stretch Bend Wag S B V B S M V M S B ALDEHYDE ALCOHOLS CARBOXYLIC ACIDS & KETONE NITRO NITRO ALIPHATIC CARBOXYLIC 1˚& 2˚AMINE PHENOLS COMPOUND COMPOUND AMINES ACID 3600 3400 3200 3000 2800 2600 2400 2200 2000 1900 1800 1700 1600 1500 1400 1300 1200 1100 1000 900 800 700 600 500 FREQUENCY/WAVENUMBER OF ABSORPTION (CM-1) Ke: S STRONG M MEDIUM W WEAK B BROAD N NARROW V VARIABLE Infrared frequencies make up a portion of the electromagnetic spectrum.
    [Show full text]