Hyphenated techniques

hyphenated technique is a combination of techniques for more advanced analysis with accurate results

1. HYPHENATED TECHNIQUES Presented By : Biji Saro Varghese M.Sc. II Sem-IV 1 RASHTRASANT TUKADOJI MAHARAJ NAGPUR UNIVERSITY P. G. T. DEPARTMENT OF CHEMISTRY 3/15/2019

2. CONTENTS INTRODUCTION GC-MS LC-MS ICP-MS MS-MS 3/15/2019 2

3. INTRODUCTION Hyphenated technique is a combination or coupling of two analytical techniques with the help of proper interface. The hyphenated technique is developed from the coupling of a separation technique and detection technique. T h e t e rm “ h y phe n at i on” was f i r st a d a p t e d b y H i rs c h f e ld i n 1980 to refer to the on-line combination of a separation technique and one or more spectroscopic detection techniques. 3/15/2019 3

4. List of hyphenated techniques GC-MS LC-MS LC-NMR EC-MS CE-MS ICP-MS GC-IR LC-MS-MS MS-MS GC-MS-MS GC-NMR GC-AES ICP-AAS 3/15/2019 4

5. Fig: Block diagram of Hyphenated technique 3/15/2019 5

6. Gas chromatography Mass spectrometry G C - M S Separates mixture of components into individual Identifies molecules based on their mass A chemical analysis technique combining two instruments to provide for powerful separation & identification . GC-MS 3/15/2019 6

7. Gas chromatography–mass spectrometry(GC-MS, or alternatively HPLC-MS) is an advanced analytical instrumental technique that combines the physical separation capabilities of gas chromatography with the mass analysis capabilities of mass spectrometer It is one of the most accurate and efficient tools for analyzing volatile organic samples. After separation in the GC column, analyte species have to be transported to the mass spectrometer to be ionized, mass filtered and detected. The column outlet needs to be connected to the ion source of the mass spectrometer and different strategies had been implemented which needs to fulfill the following conditions: Analyte must not condense in the interface. Analyte must not decompose before entering the mass spectrometer ion source. The gas load (dictated by the mobile phase gas flow rate) entering the ion source must be within the pumping capacity of the mass spectrometer. 3/15/2019 7

8. GC-MS Coupling   Direct Introduction   Jet separator   Bieman Concentrator Fig : Diagrammatic representation of GC-MS 3/15/2019 8

9. T ypes o f i n t e r f ace s : Direct Introduction 3/15/2019 9

10. Direct Introduction GC-MS systems use capillary columns & fused silica tubing permits an inert , high efficiency, direct transfer between the 2 systems. Flow rates is 5ml/min. sdfssdhjfh 3/15/2019 10

11. Jet Separator The jet separator consist of two glass tubes aligned with a Small distance between them. Carrier gas entering from the GC column is pumped away by a separate vacuumed system. The larger sample molecules maintain their momentum &pass preferentially in to the second capillary. Sample enrichment occurs & the initial atmospheric pressure is reduced . sdfssdhjfh 3/15/2019 11

12. Watson-Biemann effusion separator I t c o nsi s t s o f a s i n te r e d g l a s s t u be . The carrier gas usually helium passes preferentially through the sintered glass tube and the effluent is concentrated . T he g a s f l ow r a t e s i n the o r d e r of 2 - 60 m l/ m i n . sdfssdhjfh 3/15/2019 12

13. LC-MS L iquid chromatography-mass spectrometry is the technique which performs separation by liquid chromatography and mass analysis with the help of the mass spectrometry. Electrospray needle is used as bridge to connect the liquid chromatography with that of the mass spectrometry. LC-MS is mainly separated into the three parts- Chromatography In liquid chromatography separation is performed which is detected with the help of Photo diode Array. These separated components then transferred to the Interface. Interface In interface the liquid is volatilized and transferred to the MS . Spectrometry With the help of various ionization techniques the compound is ionized and then it is analyzed by mass analyzer. 3/15/2019 13

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15. Fig: Schematic diagram of LC-MS 3/15/2019 15

16. ICP-MS Inductively coupled plasma mass spectrometry (ICP-MS) is a type of  mass spectrometry which is capable of detecting  metals  and several  non-metals at concentrations as low as one part in 10 15  (part per quadrillion, ppq) . This is achieved by  ionizing  the sample with  inductively coupled plasma  and then using a  mass spectrometer  to separate and quantify those ions. 3/15/2019 16

17. Fig: S chematic representation of ICP-MS 3/15/2019 17

18. MS-MS Tandem In a tandem mass  spectrometer,   ions  are formed in the ion source and separated by  mass-to-charge  in the first stage of mass spectrometry (MS1). Ions of a particular mass-to-charge ratio (precursor ions) are selected and  fragment ions  (product ions) are created by  collision-induced dissociation, ion-molecule reaction, photo dissociation, or other process. The resulting ions are then separated and detected in a second stage of mass spectrometry (MS2). A common use is for analysis of biomolecules such as  proteins and   peptides. 3/15/2019 18

19. Fig :Diagrammatic representation of tandem mass spectrometry 3/15/2019 19

20. Adva n tages o f hyp h enated t e chniques Fast an d acc u rate a n alysi s . Hig h er de g r ee o f a u tom a t i o n . Hig h er sa m ple th r o u ghpu t . Be t t e r r ep r o d u c ib i l i t y . Red u c t ion o f co n tamina t i o n du e t o it s c l osed syst e m. Se p arati o n an d q u a n t i f i c a t i on ac h i e ved a t same t i me. 3/15/2019 20

21. References https :// en.wikipedia.org/wiki/Tandem_mass_spectrometry https:// en.wikipedia.org/wiki/Inductively_coupled_plasma_mass_spectrometry https:// en.wikipedia.org/wiki/Liquid_chromatography%E2%80%93mass_spectrometry https :// www.chromacademy.com/subscribe-warning.asp Trace analysis by Susanta Lahiri, Narosa Publishing House Web references 3/15/2019 21

22. THANK YOU 3/15/2019 22