mass spectroscopy

post graduate seminar

1. Ba h ir Dar University First Year M.SC In Textile Chemistry Seminar on Mass Spectroscopy and Gas Chromatography Prepared by: Asn ake Ketema 6/1/2018 Ethiopia Institute of Textile and Fashion Technology ( EiTEX

2. Mass Spectrometry Analytical method to measure the molecular or atomic weight of samples

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4. DEFINITION: Mass spectrometry (MS) is an analytical chemistry technique that helps identify the amount and type of chemicals present in a sample by measuring the mass- to-charge ratio and abundance of gas-phase ions. PRINCIPLE: A mass spectrometer generates multiple ions from the sample under investigation This molecular ion undergoes fragmentation. Each primary product ion derived from the molecular ion, in turn, undergoes fragmentation, and so on.

5. The ions are separated in the mass spectrometer according to their mass-to-charge ratio, and are detected in proportion to their abundance. A mass spectrum of the molecule is thus produced. It displays the result in the form of a plot of ion abundance versus mass-to-charge ratio

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7. Gas Chromatography 22/12/2017 8 Gas chromatography (GC) is a common technique for separating and analyzing components of a mixture.

8. Introduction Chromatography:- is a technique for separating chemical substances that relies on differences in partitioning behavior between a flowing mobile phase and a stationary phase to separate the components in a mixture. 22/12/2017 9

9. Volatility :- high‐vapor pressure or a relatively low boiling point Polarity Mechanisms Of G.C 22/12/2017 10

10. Operational Principle G .C First - a vaporized sample is injected onto the chromatographic column . Second - the sample moves through the column through the flow of inert gas. Third - the components are recorded as a sequence of peaks as they leave the column. 22/12/2017 11

11. Main Components Of G.C Carrier Ga s supply Analyst Instrument control Data acquisition Data processing Data storage Gas Flow Controller Data System Oven Column Injection Port Sample GC Detecto r 22/12/2017 12

12. 1. Carrier gas 2. Flow regulators & Flow meters 3. Injection devices 4. Columns 5. Temperature control devices 6. Detectors 7. Recorders & Integrators Practical Requirements 22/12/2017 13

13. Chromatographic Separation Mobile – inert gas used as carrier. Stationary – liquid coated on a solid or a solid within a column. 22/12/2017 14

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15. Chromatographic Analysis 1 . The number of components in a sample is determined by the number of peaks 2. The amount of a given component in a sample is determined by the area under the peaks. 3. The identity of components can be determined by the given retention times 22/12/2017 16

16. Conti . . . Peak area proportional to mass of compound injected Peak time dependent on velocity through column 22/12/2017 17 detector output

17. Applications Of G.C 1.Separation & identification of lipids , carbohydrates & proteins . 2. amino acids in urine 3. Measurement of drugs & other metabolites in biological fluids. 5. Analysis of pesticides in soil , water, food. 7. analysis of blood and urine alcohol levels 8. identify nitro-compounds in trace quantities 22/12/2017 18

18. Advantage Dis -Advantage very small samples with little preparation separating complex mixtures into components Results fast(1-100 minutes) Very high precision Equipment is not very complex. it can be easily analysis the data from the graph. Only use volatile compounds ( which can be converted in to vapor Dirty samples not give correct result 22/12/2017 19

19. Pyrolysis Gas Chromatography When the heat energy applied to the polymer chains is greater than the energy of specific bonds in that polymer chain, these bonds will fragment. 22/12/2017 seminar on Gas Chromatography 20

20. Illustrate polymer analysis by G.C protein samples shown to be useful for analysis of proteins other than wool fibers by using different special programs reflecting different amino acid compositions . acetaldehyde from alanine isobutyronitrile from valine 22/12/2017 21

21. thermally-denatured samples of wool fiber which cannot be identified successfully by morphological inspection using a microscope or by using Fourier-transform infrared micro spectroscopy. Conti . . 22/12/2017 22

22. Fibers - Cotton and Polyester PET , on the other hand, degrades to produce aromatics, including benzene, benzoic acid , and oligomeric fragments of the polymer generated from a piece of cotton thread heated to 750° C for 15 seconds . When cellulose degrades thermally, it produces water and carbon dioxide , and many other organic materials, including aldehydes and ketones . 22/12/2017 23

23. References 22/12/2017 24 Ravi Shankar, text book of pharmaceutical analysis. Skoog.D.A , Holler .F.J; principles of instrumental analysis. P.C.Kamboj ; pharmaceutical analysis- II, instrumental methods, pg.no: 281-322. P.D.Sethi ; quantitative analysis of drugs; 3rd edition. A.V.Kasture ; pharmaceutical analysis- volume II.