logging in or signing up GC- MS kalibandya Download Post to : URL : Related Presentations : Share Add to Flag Embed Email Send to Blogs and Networks Add to Channel Uploaded from authorPOINT lite Insert YouTube videos in PowerPont slides with aS Desktop Copy embed code: Embed: Flash iPad Dynamic Copy Does not support media & animations Automatically changes to Flash or non-Flash embed WordPress Embed Customize Embed URL: Copy Thumbnail: Copy The presentation is successfully added In Your Favorites. Views: 4063 Category: Science & Tech.. License: All Rights Reserved Like it (0) Dislike it (0) Added: November 23, 2011 This Presentation is Public Favorites: 3 Presentation Description GC-MS a new integrated technique that uses combined advances of GC-MS that should improve the time and efficiency of the result. Comments Posting comment... By: ranjanajaiwal (2 month(s) ago) good ppt. Saving..... Post Reply Close Saving..... Edit Comment Close By: rajkodam (9 month(s) ago) hi could u mind in giving me this ppt santosh Saving..... Post Reply Close Saving..... Edit Comment Close By: 89rohit (13 month(s) ago) plz i want this ppt my sminar topic Saving..... Post Reply Close Saving..... Edit Comment Close Premium member Presentation Transcript Gas Chromatography & Mass Spectroscopy Seminar By : Seminar Guide: Nikhil A. Khisti Prof. Deshpande (M.Pharm 1 st Sem.) (Pharma. Chemistry) : 1 23-Nov-11 1 Gas Chromatography & Mass Spectroscopy Seminar By : Seminar Guide: Nikhil A. Khisti Prof. Deshpande (M.Pharm 1 st Sem.) (Pharma. Chemistry) Gas Chromatography & Mass spectroscopy Seminar By : Nikhil A. Khisti Shital S.Bhandari Department of Pharmaceutical Chemistry AISSMS College of Pharmacy Pune-411038CONTENTS: 2 CONTENTS What is gas chromatography ? What is mass spectroscopy ? Interfacing gas chromatography with mass spectrometry History Instrumentation Application References 23-Nov-11 2What is gas chromatography ? : 3 What is gas chromatography ?  Gas chromatography is a physical separation technique applicable to volatile and thermally stable compounds which are difficult to separate and analyze. It consist of a mobile gas phase and stationary liquid phase that is coated on a solid. 23-Nov-11 3What is mass spectroscopy? : 4 What is mass spectroscopy?  Mass spectroscopy is an analytical technique capable of providing information about the structure of inorganic, organic & biological molecules; the qualitative & quantitative composition of complex mixture. In this technique molecules are bombarded with a beam of energetic electrons, to form positively charged ions which are further sorted according to their mass to charge ratio to record their masses and relative abundances. 23-Nov-11 4 History : 5 23-Nov-11 5 History  In December 1955, Roland S. Gohlke and Fred W. McLafferty coupled a home made gas chromatograph to a research time-of-flight mass spectrometer constructed by W. C. Wiley, I. H. McLaren, and D. B. Harrington. The development of affordable and miniaturized computers has helped in the simplification of the use of this instrument, as well as allowed great improvements in the amount of time it takes to analyze a sample 23-Nov-11 5 GC-MS System : 6 23-Nov-11 6 GC-MS System  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. 23-Nov-11 6Why Gas Chromatography/Mass Spectrometry? : 7 23-Nov-11 7 Why Gas Chromatography/Mass Spectrometry?  Like a good marriage, both GC & MS bring something to their union. GC can separate volatile and semi volatile compounds with great resolution, but it cannot identify them.MS can provide detailed structural information on most compounds such that they can be exactly identified, but it cannot readily separate them. GC & MS are, in many ways, highly compatible techniques. The main aim of an interfacing arrangement is to operate both GC & MS without degrading the performance of either instrument. 23-Nov-11 7Advantages : 8 23-Nov-11 8 Advantages  Enhanced sensitivity Speed Dynamic range Molecular weight Elemental composition (low MW with high resolution instrument) Structural information (hard ionization) 23-Nov-11 8How does it work? : 9 23-Nov-11 9 How does it work?  A gas chromatograph separate different types of molecules, based on their chemical properties. Resulting in each type emerging from the column in a defined sequence. The molecules would then enter the mass spectrometer, which would evaluate and identify them by breaking each one into ionized fragments and detecting these fragments using their charge-to-mass ratio. This produced a unique profile of each compound that could be converted into a digital signal and transmitted to computer 23-Nov-11 9GC MS Instrument : 10 23-Nov-11 10 GC MS Instrument  23-Nov-11 10 The insides of the GC-MS, with the column of the gas chromatograph in the oven on the right.Schematic Diagram : 11 Schematic Diagram  23-Nov-11 11Instrumentation : 12 23-Nov-11 12 Instrumentation  Parts of a Gas Chromatography: 1. Carrier Gas (N2,He) 2. Injector (Loop Inj. ,Stop flow) 3. Oven 4. Column (FSOT,SCOT) Interface between GC and MS: (Effusion, Jet/Orifice Sp) Parts of a Mass Spectroscopy: 3. Source (EI,FI,CI) 4. Mass analyzer (Quadruple Filter.) 5. Detector (electron multiplier tube) 23-Nov-11 12Carrier gases : 13 Carrier gases  Helium, Nitrogen , Argon ,Hydrogen Ideally The Carrier gas should be : * Inert * easily available * non explosive * highly pure * Suitable for detector/Sample 23-Nov-11 13Injector : 14 23-Nov-11 14 Injector  A GC syringe penetrates a septum to inject sample into the vaporization camber Instant vaporization of the sample, 280 C Carrier gas transports the sample into the head of the column Purge valve controls the fraction of sample that enters the column 23-Nov-11 14Oven : 15 23-Nov-11 15 Oven  More constant peak width Better sensitivity for components that are retained longer Much better chromatographic resolution Peak refocusing at head of column 23-Nov-11 15Open Tubular Capillary Column: 16 23-Nov-11 16 Open Tubular Capillary Column 23-Nov-11 16 0.32 mm ID Liquid Stationary phase Mobile phase (Helium) flowing at 1 mL/min 15-60 m in length 0.1-5 m mFSOT columns : 17 23-Nov-11 17 FSOT columns  Column length -10-100 m Inner Diameter - 0.1-0.53 mm Efficiency (Plates/m) - 2000-4000 Total No. of Plates - 20-400 x 10 3 Relative Speed -High Chemical Inertness -Inert for many Chemicals Flexibility -More Materials Used: Poly (phenyl methyl di methyl) siloxane (10% phenyl) Poly (phenyl methyl) siloxane (50% phenyl) Poly ethylene glycol (polar) Poly dimethyl siloxane (non-polar) 23-Nov-11 17Interface : 18 Interface  Transports the effluent from gas chromatograph to mass spectrometer Analyte must not condense in interface Analyte may not decompose before entering the mass spectrometer ion source The gas load entering the ion source must be within pumping capacity of the mass spectrometerElectron Impact  : 19 23-Nov-11 19 Electron Impact  EI (hard ionization) Gas-phase molecules enter source through heated probe or GC column 70 eV electrons bombard molecules forming M+* ions that fragment in unique reproducible way to form a collection of fragment ions EI spectra can be matched to library standards 23-Nov-11 19PowerPoint Presentation: 20 23-Nov-11 20 23-Nov-11 20 To mass analyzer filament 70 eV e- anode repeller Acceleration slits GC column EI Source Under high vacuum Quadruple Mass Ion Filter : 21 23-Nov-11 21 Quadruple Mass Ion Filter  23-Nov-11 21Steps in GC/MS analysis  : 22 Steps in GC/MS analysis  Sample preparation Derivatisation Injection GC separation Ion Formation MS Detection Scanning 23-Nov-11 22 GC-MS Video : GC-MS Video 23-Nov-11 23 23 23-Nov-11 23 APPLICATIONS: 24 23-Nov-11 24 APPLICATIONS 23-Nov-11 24PowerPoint Presentation: 25 Pharmaceuticals Pesticides Perfumery Foods Petroleum Polymers Environmental analysis 23-Nov-11 25 Biomedical Criminal forensics Textiles Clinical toxicology Explosive investigation Doping in Sport Astrochemistry Pharmaceuticals  : 26 Pharmaceuticals  separation and identification of degradation products of organic & organometallics making the elucidation of their structures. Routine analysis of substances present in minute quantities Molecular weight of pure drug To identify organic materials such as resins, fats & waxes from their chemical composition. 23-Nov-11 26Pesticide : 27 Pesticide  Identification of agrochemicals. Quantitative determination of pesticide residues in food water, etc. Quantization & conformation of organophosphorus pesticides in apple extract. Rapid screening and conformational analysis of residual pesticides in agricultural samples. 23-Nov-11 27 Perfumery & essential oils  : 28 Perfumery & essential oils  Perfumery & essential oils are very complex compound of natural origin. Each compound can contain 50 to 60 constituents or more which can be separated only by a high resolution capillary column. MS is the only means of identifying these components since it is practically impossible to get standards for them 23-Nov-11 28Foods  : 29 Foods  Analysis of flavoring compounds. Analysis of residual solvents in packing materials. Determination of residual pesticides in foods. In analysis of food, the separation & identification of lipids, proteins, carbohydrates, preservatives, colorants & texture modifiers. To analyze the dairy products for aldehydes & ketones, fatty acids & milk sugars. Analysis & Detection of 3-monochloropropane-1,2-diol in food 23-Nov-11 29Textiles : 30 Textiles  GC-MS is a very valuable tool for the detection and estimation of banned amines in dyes on the garments. Any possible banned amine in the dyes is extracted from the garment and subjected to GC-MS analysis. 23-Nov-11 30Clinical toxicology : 31 Clinical toxicology  The applicability of GC-MS for use in clinical toxicology lab was demonstrated in 1970s. One of the earliest clinical application was by Althaus who in 1970 identified propoxyphene and metabolites as agent responsible for coma in patient admitted to local hospital. Identification and confirmation of underivatized drug from extracts of urine or serum . Drug screening using GC/MS e.g. caffeine, Codeine , Methadone, Monoacetyl Morphine 23-Nov-11 31Explosive investigation  : 32 Explosive investigation  GC-MS can also be used in airport security to detect substances in luggage or on human beings. Explosive detection systems have become a part of all airports. 23-Nov-11 32Doping in Sport Symposium Proceedings  : 33 Doping in Sport Symposium Proceedings  Synthetic anabolic steroids have been in use in clinical medicine since 1940. The Analysis of Steroids in Urine Their analysis become important in 1970s, when methods for their detection were developed as part of doping control programs in athletics. A selected method is provided that allows the detection from most of the anabolic steroids (structurally related to testosterone molecule- ethylestrenol, methyl testosterone, methandienone etc) of interest in athletic doping control 23-Nov-11 33Astrochemistry  : 34 Astrochemistry  Several GC-MS have left earth. Two were brought to Mars by the Viking program. Venera 11 and 12 and Pioneer Venus , analyzed the atmosphere of Venus with GC-MS. The Huygens probe of the Cassini-Huygens mission landed one GC-MS on Saturn's largest moon, Titan. The material in the comet Gerasimenko will be analyzed by the Rosetta mission with a GC-MS in 2014. 23-Nov-11 34Limitations : 35 Limitations  Compounds with lower vapor pressures cannot be analyzed. Determining positional substitution on aromatic rings is often difficult. Certain isomeric compounds cannot be distinguished by mass spectrometry (for example, naphthalene versus azulene). MS must be tuned & calibrated before meaning full data can be obtained. Requires computer with large storage system. Expensive than others. Interpretation of result requires highly trained personsReferences: 36 23-Nov-11 36 References Willard H., Merritt L., Dean J., Settle F., Instrumental methods of Analysis .7 th Edition, CBS Publisher & Distributors, 1986, New Delhi, 480, 540-544,569-572 J Mendham R.C. Denney J.D. Barnes M Thomas. Vogel’s Textbook of Quantitative Chemical Analysis . 6 th Edition, Pearson Education, 2005, 350 Skoog D., Holler F., Niemen T., Principles of Instrumental Analysis. 5 th Edition, Thomson Books, 2005, 718-720 McMaster M., McMaster C., GC/MS A Practical User’s Guide. 1 st Edition, WILEY-VCH publication,1998, 4-10 Frost R.,Gautier D., Journal Of Analytical Technology. 2006, 30 (3), 210-215 Chatwal G., Anand S., Instrumental Methods of Chemical Analysis. 5 th edition, Himalaya publication house, 2006, 2.691-2.699. 23-Nov-11 36PowerPoint Presentation: 37 23-Nov-11 37 Ellis L. and Fincannon A, Organic Geochemistry. 1998, 29 (5-7), 1101-1117 Müller A., Düchting P., Weiler E., Planta. 2002, 216(1), 44-56. Min An, Pratley J., Haig T., Rapid Communications in Mass Spectrometry. 1998,10 (1), 104 - 105 http://en.wikipedia.org/wiki/Gas_chromatography-mass_spectrometry (accessed 14/10/2008) . http://www.chemsoc.org/ExemplarChem/entries/2004/westengland_smith/ExempWeb/GC-MS.htm. (accessed14/10/2008) http://en.wikipedia.org/wiki/Gas _chromatography-mass _spectroscopy.” (accessed 14/10/2008) http://www.kcl.ac.uk/ms-facility/gcms.html. (accessed 12/10/2008) http://www.gmu.edu/departments/SRIF/tutorial/gcd/gc-ms2.html. (accessed 12/10/2008) http://www.gmu.edu/departments/SRIF/tutorial/gcd/pc..html (accessed 13/10/2008) 23-Nov-11 37PowerPoint Presentation: 38 23-Nov-11 38 http://www.science24.com/paper/6544 (accessed 14/10/2008) http://www.ncbi.nlm.nih.gov/pubmed/15733837 (accessed 14/10/2008) http://pubs.acs.org/cgi-bin/abstract.cgi/ancham/1973/45/i06/f-pdf/f_ac60328a006.pdf?sessid=6006l3 (accessed 14/10/2008) http://www.prenhall.com/settle/chapters/ch31.pdf (accessed 14/10/2008) http://www.chem.vt.edu/chem-ed/sep/gc/gc.html. (accessed 14/10/2008) http://www.clu-in.org/download/techdrct/tdmpa_gc- ms_report.pdf. (accessed 14/10/2008) http://fate.clu-in.org/gc.asp?techtypeid=44 (accessed14/10/2008) http://www.chem.vt.edu/chem-ed/ms/ms-intro.html. (accessed 14/10/2008) http://caag.state.ca.us/bfs/toxlab/gcms.html. (accessed 14/10/2008)PowerPoint Presentation: 39 23-Nov-11 39 THANK YOU You do not have the permission to view this presentation. In order to view it, please contact the author of the presentation.