Chromatography and Separation Science 2003 – Ahuja
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Gas Chromatography-Mass Spectroscopy
Gas Chromatography-Mass Spectroscopy Introduction Gas chromatography-mass spectroscopy (GC-MS) is one of the so-called hyphenated analytical techniques. As the name implies, it is actually two techniques that are combined to form a single method of analyzing mixtures of chemicals. Gas chromatography separates the components of a mixture and mass spectroscopy characterizes each of the components individually. By combining the two techniques, an analytical chemist can both qualitatively and quantitatively evaluate a solution containing a number of chemicals. Gas Chromatography In general, chromatography is used to separate mixtures of chemicals into individual components. Once isolated, the components can be evaluated individually. In all chromatography, separation occurs when the sample mixture is introduced (injected) into a mobile phase. In liquid chromatography (LC), the mobile phase is a solvent. In gas chromatography (GC), the mobile phase is an inert gas such as helium. The mobile phase carries the sample mixture through what is referred to as a stationary phase. The stationary phase is usually a chemical that can selectively attract components in a sample mixture. The stationary phase is usually contained in a tube of some sort called a column. Columns can be glass or stainless steel of various dimensions. The mixture of compounds in the mobile phase interacts with the stationary phase. Each compound in the mixture interacts at a different rate. Those that interact the fastest will exit (elute from) the column first. Those that interact slowest will exit the column last. By changing characteristics of the mobile phase and the stationary phase, different mixtures of chemicals can be separated. -
Qualitative and Quantitative Analysis
qualitative and quantitative analysis Russian scientist Tswett in 1906 used a glass columns packed with divided CaCO3(calcium carbonate) to separate plant pigments extracted by hexane. The pigments after separation appeared as colour bands that can come out of the column one by one. Tswett was the first to use the term "chromatography" derived from two Greek words "Chroma" meaning color and "graphein" meaning to write. Invention of Chromatography by M. Tswett Ether Chromatography Colors Chlorophyll CaCO3 5 *Definition of chromatography *Tswett (1906) stated that „chromatography is a method in which the components of a mixture are separated on adsorbent column in a flowing system”. *IUPAC definition (International Union of pure and applied Chemistry) (1993): Chromatography is a physical method of separation in which the components to be separated are distributed between two phases, one of which is stationary while the other moves in a definite direction. *Principles of Chromatography * Any chromatography system is composed of three components : * Stationary phase * Mobile phase * Mixture to be separated The separation process occurs because the components of mixture have different affinities for the two phases and thus move through the system at different rates. A component with a high affinity for the mobile phase moves quickly through the chromatographic system, whereas one with high affinity for the solid phase moves more slowly. *Forces Responsible for Separation * The affinity differences of the components for the stationary or the mobile phases can be due to several different chemical or physical properties including: * Ionization state * Polarity and polarizability * Hydrogen bonding / van der Waals’ forces * Hydrophobicity * Hydrophilicity * The rate at which a sample moves is determined by how much time it spends in the mobile phase. -
Fractionation of Proteins with Two-Sided Electro-Ultrafiltration
Journal of Biotechnology 128 (2007) 895–907 Fractionation of proteins with two-sided electro-ultrafiltration Tobias Kappler¨ ∗, Clemens Posten University of Karlsruhe, Institute of Engineering in Life Sciences, Division Bioprocess Engineering, Kaiserstr. 12, Geb. 30.70, 76128 Karlsruhe, Germany Received 7 June 2006; received in revised form 22 December 2006; accepted 2 January 2007 Abstract Downstream processing is a major challenge in bioprocess industry due to the high complexity of bio-suspensions itself, the low concentration of the product and the stress sensitivity of the valuable target molecules. A multitude of unit operations have to be joined together to achieve an acceptable purity and concentration of the product. Since each of the unit operations leads to a certain product loss, one important aim in downstream-research is the combination of different separation principles into one unit operation. In the current work a dead-end membrane process is combined with an electrophoresis operation. In the past this concept has proven successfully for the concentration of biopolymers. The present work shows that using different ultrafiltration membranes in a two-sided electro-filter apparatus with flushed electrodes brought significant enhancement of the protein fractionation process. Due to electrophoretic effects, the filtration velocity could be kept on a very high level for a long time, furthermore, the selectivity of a binary separation process carried out exemplarily for bovine serum albumin (BSA) and lysozyme (LZ) could be greatly increased; in the current case up to a value of more than 800. Thus the new two-sided electro-ultrafiltration technique achieves both high product purity and short separation times. -
Laser Desorption/Ionization Time-Of-Flight Mass Spectrometry of Biomolecules Yu-Chen Chang Iowa State University
Iowa State University Capstones, Theses and Retrospective Theses and Dissertations Dissertations 1996 Laser desorption/ionization time-of-flight mass spectrometry of biomolecules Yu-chen Chang Iowa State University Follow this and additional works at: https://lib.dr.iastate.edu/rtd Part of the Analytical Chemistry Commons Recommended Citation Chang, Yu-chen, "Laser desorption/ionization time-of-flight mass spectrometry of biomolecules " (1996). Retrospective Theses and Dissertations. 11366. https://lib.dr.iastate.edu/rtd/11366 This Dissertation is brought to you for free and open access by the Iowa State University Capstones, Theses and Dissertations at Iowa State University Digital Repository. It has been accepted for inclusion in Retrospective Theses and Dissertations by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. INFORMATION TO USERS This manuscript has been rqjroduced fix>m the microfihn master. UMI fihns the text directly from the original or copy submitted. Thus, some thesis and dissertation copies are in typewriter face, w^e others may be from any type of computer printer. The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleedthrough, substandard margins, and improper alignment can adversely afifect reproduction. In the unlikely event that the author did not send IMl a complete manuscript and there are misang pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. Oversize materials (e.g., maps, drawings, charts) are reproduced by sectioning the original, beginning at the upper left-hand comer and continuing from left to right in equal sections with small overlaps. -
Separations Development and Application (WBS 2.4.1.101) U.S
Separations Development and Application (WBS 2.4.1.101) U.S. Department of Energy (DOE) Bioenergy Technologies Office (BETO) 2017 Project Peer Review James D. (“Jim”) McMillan NREL March 7, 2017 Biochemical Conversion Session This presentation does not contain any proprietary, confidential, or otherwise restricted information. Project Goal Overall goal: Define, develop and apply separation processes to enable cost- effective hydrocarbon fuel / precursor production; focus on sugars and fuel precursor streams; lipids pathway shown. Outcome: Down selected proven, viable methods for clarifying and concentrating the sugar intermediates stream and for recovering lipids from oleaginous yeast that pass “go” criteria (i.e., high yield, scalable, and cost effective). Relevance: Separations are key to overall process integration and economics; often represent ≥ 50% of total process costs; performance/efficiency can make or break process viability. Separations this project investigates – sugar stream clarification and concentration, and recovery of intracellular lipids from yeast – account for 17-26% of projected Minimum Fuel Selling Price (MFSP) for the integrated process. 2 Project Overview • Cost driven R&D to assess/develop/improve key process separations - Sugar stream separations: S/L, concentrative and polishing - Fuel precursor recovery separations: oleaginous yeast cell lysis and LLE lipid recovery • Identify and characterize effective methods - Show capability to pass relevant go/no-go criteria (e.g., high yield, low cost, scalable) • Exploit in situ separation for process intensification - Enable Continuous Enzymatic Hydrolysis (CEH) • Generate performance data to develop / refine process TEAs and LCAs 3 Separations Technoeconomic Impact $1.78 $2.18 $1.43 $0.79 4 Quad Chart Overview Timeline Barriers Primary focus on addressing upstream and Start: FY 15 (Oct., ‘14) downstream separations-related barriers: End: FY 17 (Sept., ‘17; projected) – Ct-G. -
Rubber-Modified Epoxies: in Situ Detection of the Phase Separation by Differential Scanning Calorimetry
Rubber-modified epoxies: in situ detection of the phase separation by differential scanning calorimetry Dong Pu Fang*, C. C. Riccardi and R. J. J. Williamst Institute of Materials Science and Technology (INTEMA), University of Mar de/Plata and National Research Council (CONICET), J. B. Justo 4302, 7600 Mar de/Plata, Argentina (Received 18 May 1993) The phase separation of a rubber in the course of a thermosetting polymerization is associated with heat release. Mixing is endothermic as revealed by the positive value of the interaction parameter while demixing is exothermic. Differential scanning calorimetry may be used to detect heat effects related to phase separation. Experimental results are reported for an unreactive system (castor oil/epoxy resin) and reactive systems (modifier/epoxy resin/diamine) using either castor oil or epoxy-terminated copolymers of acrylonitrile and butadiene as modifiers. (Keywords: rubber-modified epoxies; phase separation; d.s.c.) Introduction represents the residual free energy of mixing (part or all A common method to toughen epoxy resins is to of it may be considered as an enthalpic contribution). dissolve rubbers or other modifiers that become phase- The interaction parameter A, expressed in units of energy separated in the course of polymerization. The resulting per unit volume, is usually a positive value. This means two-phase structure exhibits an increase in the fracture that mixing occurs due to the prevailing influence of the resistance at the expense of lower values of the elastic combinatorial part of the equation over the interaction modulus and yield stress. term. Dissimilar molecules (positive A) are thus obliged Monitoring the phase separation process is important to mix due to an entropic driving force; their intrinsic in two respects: (i) for unreactive epoxy-rubber repulsion is manifested by an endothermic effect in the formulations, i.e. -
Distillation Accessscience from McgrawHill Education
6/19/2017 Distillation AccessScience from McGrawHill Education (http://www.accessscience.com/) Distillation Article by: King, C. Judson University of California, Berkeley, California. Last updated: 2014 DOI: https://doi.org/10.1036/10978542.201100 (https://doi.org/10.1036/10978542.201100) Content Hide Simple distillations Fractional distillation Vaporliquid equilibria Distillation pressure Molecular distillation Extractive and azeotropic distillation Enhancing energy efficiency Computational methods Stage efficiency Links to Primary Literature Additional Readings A method for separating homogeneous mixtures based upon equilibration of liquid and vapor phases. Substances that differ in volatility appear in different proportions in vapor and liquid phases at equilibrium with one another. Thus, vaporizing part of a volatile liquid produces vapor and liquid products that differ in composition. This outcome constitutes a separation among the components in the original liquid. Through appropriate configurations of repeated vaporliquid contactings, the degree of separation among components differing in volatility can be increased manyfold. See also: Phase equilibrium (/content/phaseequilibrium/505500) Distillation is by far the most common method of separation in the petroleum, natural gas, and petrochemical industries. Its many applications in other industries include air fractionation, solvent recovery and recycling, separation of light isotopes such as hydrogen and deuterium, and production of alcoholic beverages, flavors, fatty acids, and food oils. Simple distillations The two most elementary forms of distillation are a continuous equilibrium distillation and a simple batch distillation (Fig. 1). http://www.accessscience.com/content/distillation/201100 1/10 6/19/2017 Distillation AccessScience from McGrawHill Education Fig. 1 Simple distillations. (a) Continuous equilibrium distillation. -
Advanced Separation Techniques Combined with Mass Spectrometry for Difficult Analytical Tasks - Isomer Separation and Oil Analysis
FINNISH METEOROLOGICAL INSTITUTE Erik Palménin aukio 1 P.O. Box 503 FI-00101 HELSINKI 131 CONTRIBUTIONS tel. +358 29 539 1000 WWW.FMI.FI FINNISH METEOROLOGICAL INSTITUTE CONTRIBUTIONS No. 131 ISBN 978-952-336-016-7 (paperback) ISSN 0782-6117 Erweko Helsinki 2017 ISBN 978-952-336-017-4 (pdf) Helsinki 2017 ADVANCED SEPARATION TECHNIQUES COMBINED WITH MASS SPECTROMETRY FOR DIFFICULT ANALYTICAL TASKS - ISOMER SEPARATION AND OIL ANALYSIS JAAKKO LAAKIA Department of Chemistry University of Helsinki Finland Advanced separation techniques combined with mass spectrometry for difficult analytical tasks – isomer separation and oil analysis Jaakko Laakia Academic Dissertation To be presented, with the permission of the Faculty of Science of the University of Helsinki, for public criticism in Auditorium A129 of the Department of Chemistry (A.I. Virtasen aukio 1, Helsinki) on May 12th, 2017, at 12 o’clock noon. Helsinki 2017 1 TABLE OF CONTENTS ABSTRACT 4 Supervisors Professor Tapio Kotiaho TIIVISTELMÄ 5 Department of Chemistry LIST OF ORIGINAL PAPERS 6 Faculty of Science ACKNOWLEDGEMENTS 7 ABBREVIATIONS 8 and 1. INTRODUCTION 10 Division of Pharmaceutical Chemistry and Technology 1.1.1 Basic operation principles of ion mobility 12 spectrometry 11 Faculty of Pharmacy 1.1.2 Applications of ion mobility spectrometry 16 University of Helsinki 1.2 Basic operation principles and applications of two-dimensional gas 19 chromatography – time-of-flight mass spectrometry Docent Tiina Kauppila 1.3 Aims of study 23 Division of Pharmaceutical Chemistry and Technology -
Removal of Waterborne Particles by Electrofiltration: Pilot-Scale Testing
ENVIRONMENTAL ENGINEERING SCIENCE Volume 26, Number 12, 2009 ª Mary Ann Liebert, Inc. DOI: 10.1089=ees.2009.0238 Removal of Waterborne Particles by Electrofiltration: Pilot-Scale Testing Ying Li,1 Ray Ehrhard,1 Pratim Biswas,1,* Pramod Kulkarni,2 Keith Carns,3 Craig Patterson,4 Radha Krishnan,5 and Rajib Sinha5 1Department of Energy, Environmental and Chemical Engineering, Washington University in St. Louis, St. Louis, Missouri. 2Center for Disease Control and Prevention, National Institute for Occupational Safety and Health, Cincinnati, Ohio. 3Global Energy Partners, LLC, Oakhurst, California. 4Office of Research and Development, National Risk Management Research Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. 5Shaw Environmental and Infrastructure, Inc., Cincinnati, Ohio. Received: July 6, 2009 Accepted in revised form: October 20, 2009 Abstract Theoretical analysis using a trajectory approach indicated that in the presence of an external electric field, charged waterborne particles are subject to an additional migration velocity that increases their deposition on the surface of collectors (e.g., sand filter). Although researchers conducted bench-scale experiments to verify the effectiveness of electrofiltration, few studies have reported on the applications of electrofiltration in larger scale facilities. In this study, a prototype pilot-scale electrofiltration unit, consisting of an acrylic tank (0.3Â0.3Â1.2 m) with vertically placed stainless steel mesh electrodes embedded in a sand filter was tested at a local drinking water plant. Presedimentation basin water was used as the influent with a turbidity ranging from 12 to 37 NTU. At an approach velocity of 0.84 mm=s, an electrode voltage at 8 and 12 V increased the particle removal coefficient pC* [defined as Àlog(Cout=Cin)] to 1.79 and 1.86, respectively, compared to 1.48 when there was no electric field. -
Chem Tech Pro 2F/20, Jaljyoti Appartment, New Sama Road, Chhani Jakat Naka, Vadodara-390002 Website: Email: [email protected]
Suppliers of all types of Equipments, Instruments and Chemicals Hub for all types Equipments, Instruments and Chemicals for various industries Registered Marketing Office: Chem Tech Pro 2F/20, Jaljyoti Appartment, New Sama Road, Chhani Jakat Naka, Vadodara-390002 Website: www.chemtechpro.in Email: [email protected] 1 About Chem Tech Pro Chem Tech Pro is global leading suppliers of various scientific equipments, chemical equipments, educational equipments, pilot plants for chemicals and pharmaceuticals products, analytical instruments, automation systems, labo- ratory chemicals, industrial chemicals and varieties of technical services pro- vider. Chem Tech Pro’s Products and Services 1. Absorption Columns 2. Adsorption Columns 3. Agitators 4. Analytical Equipments 5. Boilers and Steam Generators 6. Catalysts 7. Centrifuges 8. Chemicals 9. Cooling Towers 10. Crystallizers 11. Decanters 12. Distillation Columns 13. Dryers 14. Educational Equipments for Engineering Colleges 15. Environmental Equipments 16. Evaporators 17. Extraction Units 18. Fans, Blowers and Compressors 19. Fermenters and Bioreactors 20. Furnaces 21. Glass Equipments 22. Heat Exchangers 23. Humidifiers 24. Ion Exchange Equipments 25. Liquid Handling Equipments 26. Material Handling Equipments 27. Mechanical Seals and Stuffing Boxes 28. Membrane and Filtration Equipments 29. Mixing and Blending Units 30. Packing for columns 31. Personal Protective Equipments 32. Pilot Plants Specialists 33. Polymers 34. Pressure Vessels 35. Process Controllers and Instruments 36. Pumps 37. Reactors 38. Re-boilers 39. Safety and Fire fighting Equipments 40. Sewage Treatment Plants 41. Sight Glass and Flow Indicators 42. Solar Equipments 43. Sonicators and Homogenizers 44. Storage Tanks 45. Surface Treatment Equipments 46. Technical Services for various industries 47. Thickeners and Clarifiers 48. -
Lithium Isotope Separation a Review of Possible Techniques
Canadian Fusion Fuels Technology Project Lithium Isotope Separation A Review of Possible Techniques Authors E.A. Symons Atomic Energy of Canada Limited CFFTP GENERAL CFFTP Report Number s Cross R< Report Number February 1985 CFFTP-G-85036 f AECL-8 The Canadian Fusion Fuels Technology Project represents part of Canada's overall effort in fusion development. The focus for CFFTP is tritium and tritium technology. The project is funded by the governments of Canada and Ontario, and by Ontario Hydro. The Project is managed by Ontario Hydro. CFFTP will sponsor research, development and studies to extend existing experience and capability gained in handling tritium as part of the CANDU fission program. It is planned that this work will be in full collaboration and serve the needs of international fusion programs. LITHIUM ISOTOPE SEPARATION: A REVIEW OF POSSIBLE TECHNIQUES Report No. CFFTP-G-85036 Cross Ref. Report No. AECL-8708 February, 1985 by E.A. Symons CFFTP GENERAL •C - Copyright Ontario Hydro, Canada - (1985) Enquiries about Copyright and reproduction should be addressed to: Program Manager, CFFTP 2700 Lakeshore Road West Mississauga, Ontario L5J 1K3 LITHIUM ISOTOPE SEPARATION: A REVIEW OF POSSIBLE TECHNIQUES Report No. OFFTP-G-85036 Cross-Ref Report No. AECL-87O8 February, 1985 by E.A. Symons (x. Prepared by: 0 E.A. Symons Physical Chemistry Branch Chemistry and Materials Division Atomic Energy of Canada Limited Reviewed by: D.P. Dautovich Manager - Technology Development Canadian Fusion Fuels Technology Project Approved by: T.S. Drolet Project Manager Canadian Fusion Fuels Technology Project ii ACKNOWLEDGEMENT This report has been prepared under Element 4 (Lithium Compound Chemistry) of the Fusion Breeder Blanket Program, which is jointly funded by AECL and CFFTP. -
Enrichment of Natural Products Using an Integrated Solvent-Free Process: Molecular Distillation
BK1064-ch62_R2_250706 SYMPOSIUM SERIES NO. 152 # 2006 IChemE ENRICHMENT OF NATURAL PRODUCTS USING AN INTEGRATED SOLVENT-FREE PROCESS: MOLECULAR DISTILLATION Fregolente, L.V.; Moraes, E.B.; Martins, P.F.; Batistella, C.B.; Wolf Maciel, M.R.; Afonso, A.P.; Reis, M.H.M. Chemical Engineering School/Separation Process Development Laboratory (LDPS) State University of Campinas – CP 6066 – CEP 13081-970 – Campinas – SP – Brazil E-mail: [email protected] Molecular distillation is a potential process for separation, purification and/or concentration of natural products, usually constituted by complex and thermally sen- sitive molecules, such as vitamins. Furthermore, this process has advantages over other techniques that use solvents as the separating agent, avoiding problems of toxi- city. This process is characterized by short exposure of the distilled liquid to high temperatures, by high vacuum (around 1024 mmHg) in the distillation space and by a small distance between the evaporator and the condenser (around 2 cm). The pro- ductivity of the process is high, considering the concentration of high added value compounds. In this work, the molecular distillation process was applied to enrich borage oil in gamma-linolenic acid (GLA) and also to recover tocopherols from deo- dorizer distillate of soybean oil (DDSO), since these are components of interest for food and pharmaceutical industries. KEYWORDS: gamma-linolenic acid, vitamin E, molecular distillation, deodorizer distillate of soybean oil, borrage oil INTRODUCTION Molecular distillation shows potential in the separation, purification and/or concentration of natural products, usually constituted by complex and thermally sensitive molecules, such as vitamins and polyunsaturated fatty acids, because it can minimize losses by thermal decomposition.