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Gerstel 頂空進樣 Headspace MPS 三合一系統 ( 液體,頂空, SPME) Page 2.

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Presentation on theme: "Gerstel 頂空進樣 Headspace MPS 三合一系統 ( 液體,頂空, SPME) Page 2."— Presentation transcript:

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2 Gerstel 頂空進樣 Headspace

3 MPS 三合一系統 ( 液體,頂空, SPME) Page 2

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5 l Supports mutliple injection ports l Syringe-only concept l Modular l Saves bench space l Highly adaptable l Fully controlled through the advanced MASter software

6 l 3 Sample trays: - 98 x 2 ml Vials - 200 x 1 ml Vials - 32 x 10/20 ml Vials l Universal syringe holder for syringes from 10 µl up to 1000 µl

7 l Liquid injections from 1 µl up to 1000 µl in conjunction with a CIS l Large Volume Calculator l Injection speed programmable l Lower detections limits

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9 l Multiple Headspace Extraction in conjunction with GERSTEL-ColdInjectionSystems l Syringe Headspace Injections l Syringeholder heatable up to 150° C l Hot Needle Injection l 3 sample trays : 98 x 2 ml Vials 32 x 10/20 ml Vials l Agitator for 6 samples

10 l Automated Solid-Phase-Micro-Extraction (SPME) l Liquid and Headspace SPME possible l 3 sample trays : 98 x 2 ml Vials 32 x 10/20 ml Vials l Thermal sample equilibration and agitation l For all common SPME fibers l Bake out station for SPME fibers

11 l Dilute l Extractions l Derivatisation l Adding internal standards

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14 應用 Page 13

15 Page 14 其他應用 ( 以下為一些資料的應用 ) Traditional HSS Applications  Forensic: Blood Alcohol Analysis  Pharmaceutical: Residual Solvent Analysis (USP 467, EP)  Environmental: VOC in Drinking Water  Consumer Products: Flavor and Fragrance New Application Extension  High Temp. Polymer  Semi-volatile active compounds: Pesticides Analysis

16 Page 15 Blood Alcohol - Dual Column Confirmation GC Oven:35 o C isothermal Inlet:Split/Splitless at 150 o C *a two-hole ferrule (p/n 5062-3580) was used to connect both columns to the same inlet Column I: DB-ALC1 (p/n 123-9134) 30 m x 0.32 mm x 1.8 µm Column II:DB-ALC2 (p/n 123-9234) 30 m x 0.32 mm x 1.2 µm Headspace oven: 60 o C Vial equilibration time: 15 min. Sample: 5ul of 0.08 g/dL standard mix in 10 ml vial 1.Acetaldehyde 2.Methanol 3.Ethanol 4.Acetone 5.2-Propanol 6.Acetonitrile 7.Ethyl Acetate 8.Methyl-Ethyl Ketone 1.002.003.004.005.00 Column I 1.002.003.004.005.00 Column II 1 2 3 4 5 6 7 8 12 3 4, 6 5 7 8

17 G1888 Sales Training Jan. 2004 Agilent Restricted Page 16 Residual Solvent in Pharmaceutical Product min 02468 101214 1 15 7 17 19 20 1 22 21 18 16 2 3 4 5 6 13,14 12 8 9 11 10 Headspace Conditions: Oven Temp: 85 o C Loop Temp: 95 o C Transfer Line Temp: 110 o C Vial equilibration time: 10 min GC Condition: Column: DB-624, 30 m x 0.53 mm x 3.0 um Carrier: Helium, 35 cm/sec, Constant Flow Oven: 40 o C (5 min) to 90 o C at 2 o C/min 90 o C to 250 o C at 30 o C/min Injection: Headspace, 180 o C, Split 7/1 Detector: FID, 260 o C 1 Methanol 2 Ethanol 3 Ether 4 Acetone 5 i - Propanol 6 Acetonitrile 7 Methylene Chloride 8 t - Butanol 9 Hexane 10 Propanol 11 Methylethylketone 12 Ethylacetate 13 Tetrahydrofuran 14 s - Butanol 15 Chloroform 16 Cyclohexane 17 Benzene 18 Heptane 19 Trichloroethylene 20 1,4 - Dioxane 21 Pyridine 22 Toluene

18 Page 17 VOC in Water – HS/GC/MSD Application 2.004.006.008.0010.0012.0014.0016.00 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 293031 Sample: 40 ppb, 5ml water in 10 ml vial, 2 grams NaCl added Column: 20 m x 0.18 mm x 1.0 DB-VRX (PN: 121-1524) Headspace oven temp: 75 o C Equilibration time: 20 min MSD Scan range: 45 – 260 amu 1. Chloromethane, 2.Vinyl chloride, 3. Bromomethane, 4. Chloroethane, 5.Trichloromonofluoromethane, 6. 1,1 Dichloroethene, 7. Methylene chloride, 8. 1,2 dichloroethane, 9. Trichloromethane, 10. 1,2 dichloroethane, 11. 1,1,1 Trichloroethane, 12. Carbon tetrachloride, 13. Benzene, 14. 1,2 dichloropropane, 15. Trichloroethylene, 16. Bromodichloromethane, 17. 2 chloroethoxyethane, 18. cis 1,3 dichloropropene, 19. trans 1,3 dichloropropene, 20. 1,1,2 trichloroethane, 21. Toluene, 22. Dibromochloromethane, 23. Tetrachloroethylene, 24. Chlorobenzene, 25. Ethylbenzene, 26. Bromoform, 27. 1,1,2,2 tetrachloroethane, 28. 1,3 dichlorobenzene, 29. 1,4 dichlorobenzene, 30. 1,2 dichlorobenzene

19 Page 18 High Temp: Soda Bottle – PET Analysis (new) Column: 30 m x 0.25 mm x 0.5 HP-5MS (PN 19091S-133) Headspace equilibration time: 30 min MSD Scan range: 35 – 250 amu Sample: 0.5cm x 0.5 cm squares of soda bottle, 2.0 g in 20 ml vial under nitrogen 4.006.008.0010.0012.0014.0016.0018.0020.0022.0024.0026.0028.0030.00 123 4 5 6 7 5.0010.0015.0020.0025.0030.0035.0040.0045.0050.00 55.00 21 3 4 5 6 7 HSS Temp 100 o C HSS Temp. 230 o C 1. Propylene glycol n-propylether, 2. Diketone alcohol, 3. Mycene, 4. Octanol, 5. D-Limonene, 6. Terpinene, 7. Nonanal, 8. Decanal 1. Methyldioxolane, 2. Ethylene glycol, 3. Hydroxy ethylacetate, 4. Methylester acetic acid, 5. D-limonene, 6. Decanal, 7. n-Hexadecanoic acid

20 G1888 Sales Training Jan. 2004 Agilent Restricted Page 19 Pesticide Analysis (HS/GC/MSD/VI inlet) (new) Sample: 100 ng Pesticide mix in Acetone Full evaporation method, ~ 1 ng on column injected Column: 30 m x 0.25 mm x 0.25um HP-5MS GC: 6890N with volatiles interface, Split 5 to 1 MSD: 5973 inert HSS: G1888A Conditions 10 ml vial Temp: 225 o C, 15 min. 10.0015.0020.0025.0030.00 35.00 1 2 3 4 5 6 7 8 9 10 11 12 13 1415 16 17 18 19 20 21 22 23 24 25 26 27 1. Dichlorvos 3. Vernolate 8. Lindane 15. Chlorpyrifos 17. P,p’-DDE 19. Propargite 21. Mirex 27. Fluvalinate

21 Page 20 Perfume Base for Consumer Products 5.0010.0015.0020.0025.0030.0035.00 1 2 3 4 5 Headspace conditions: Temp: 100 o C Equilibrium Time 30 min Evaporation method, 3 drops in 10 ml vial MSD: 5973 inert, scan 30 – 500 amu GC: 6890N with volatiles interface Column: 30 m x 0.25 mm x 0.5um HP-5MS 1.Pinene, 2.2,6 dimethyl 7-Octen-2-ol, 3.Phenylmethylester acetic acid 4.Vertenex, 5.Hexylsalicylate

22 Page 21 Brewed Coffee 1. Acetaldehyde, 2. Acetone, 3. 2-methyl propanal, 4. 4. 2-butanone, 5. 2-methyl furan 6. Acetic acid, 7. 3-methyl butanal, 8. 2-methyl butanal 1.001.502.002.503.003.504.004.505.005.50 1 2 3 4 5 6 78 Headspace Conditions: Temp: 80 o C Time: 30 min Sample: 10 ml coffee in 20 ml vial MSD: 5973 inert, scan 30 – 300 amu GC: 6890N with volatiles interface

23 Page 22 Orange Oil 5.0010.0015.0020.0025.0030.00 1 2 3 4 5 6 7 8 9 Column: 30 m x 0.25 mm x 0.50 HP-5MS Headspace oven temp: 100 o C Equilibration time: 20 min MSD Scan range: 35 – 260 amu Sample: 3 drops orange oil in 10ml vial 1. Dimethylvinylmethanol 2. nonane, 3. Pinene, 4. Phellandrene, 5. Myrcene, 6. Limonene, 7. 1-Octanol, 8. Linalool 9. Decanal

24 Page 23 Rose Oil 50.00 3 5.0010.0015.0020.0025.0030.0035.0040.0045.00 1 2 4 5 6 7 MSD OFFElution of phenylethyl alcohol Headspace Conditions: Temp: 225 o C Time: 30 min. Evaporation method, 3 drops in 10 ml vial MSD: 5973 inert, scan 30 –300 amu GC: 6890N with volatiles interface 1. Dimethylvinylmethanol 2. nonane, 3. Pinene, 4. Phellandrene, 5. Myrcene, 6. Limonene, 7. 1-Octanol, 8. Linalool 9. Decanal


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