SUPELCO. Improved Performance for Cyanopropylphenyldimethylpolysiloxane (SPB-1701, SPB-1301) Capillary Columns

Transcription

1 Improved Performance for Cyanopropylphenyldimethylpolysiloxane (SPB-1701, SPB-1301) Capillary Columns L.M. Sidisky, Yizeng Ni, Greg Baney, Rodney George, Katherine K. Stenerson T CFK

2 Discussion Topics Introduction Phase Chemistry/ Composition Polarity Comparison Bleed Comparison Applications Summary

3 Possible Structures for 1701 Phase Me Ph Si O Si O Me x Cp y Me Ph Cp Si O Si O Si O Me Me x y Me z Me Me Me Cp Si O Si Si O Si O Me Me Me Me x y z Cp=Cyanopropyl

4 Typical Phase Composition % Methyl % Phenyl % Cyano Competitor A Competitor B Competitor C Silphenylene SPB

5 KRI Polarity Comparison Average KRI values for 2-Octanone Competitor A Competitor B Competitor C Silphenylene SPB

6 Selectivity Difference 30m x 0.25mm ID x 0.25µm Competitor C SPB

7 Discussion Topics Introduction Phase Chemistry/Composition Polarity Comparison Bleed Comparison Applications Summary

8 Competitor A: 30m x 0.25mm ID x 0.25µm Bleed 46 pa at 280 o C

9 Competitor B: 30m x 0.25mm ID x 0.25µm Bleed 280 o C 25 pa 20 pa 67 pa

10 SPB-1701: 30m x 0.25mm ID x 0.25µm Bleed 280 o C

11 Discussion Topics Introduction Phase Chemistry/ Composition Polarity Comparison Bleed Comparison Applications Summary

12 Peak Symmetry on SPB Blood Alcohols Conditions: Column: 30m x 0.25mm ID, 0.25µm Oven: Inj.: Det.: Flow: 40 o C, (5 min.) 4 o C/min to 100 o C 200 o C FID, 250 o C 20cm/sec He at 40 o C Injection: 1.0µL, 100:1 split Sample: 0. 5µL/mL in water Peak ID: 1. Acetaldehyde 2. Methanol 3. Ethanol 4. Acetone 5. Isopropanol 6. n-propanol Better peak symmetry, for improved resolution... SPB-1701 Competitor B Blood Alcohols Analysis Better response on later eluting compounds... 6 Increased tailing on competitor column min. 4 min. 5 min

13 Organochlorine Pesticides on a 30m x 0.53mm ID, 0.50µm Column

14 Organochlorine Pesticides on SPB-1701 Peak ID: 1. Tetrachloro-m-xylene 2. α-bhc 3. γ-bhc 4. Heptachlor 5. Aldrin 6. β-bhc 7. δ-bhc 8. Heptachlor Epoxide 9. Endosulfan I 10. γ-chlordane 11. α -Chlordane 12. 4,4 -DDE 13. Dieldrin 14. Endrin 15. 4,4 -DDD 16. Endosulfan II 17. 4,4 -DDT 18. Endrin Aldehyde 19. Methoxychlor 20. Endosulfan sulfate 21. Endrin ketone 22. Decachlorobiphenyl Heptachlor Conditions: Column: 30m x 0.53mm ID, 1.0µm Flow: 28cm/sec He at 150 o C Oven: 150 o C, 4 o C/min to 275 o C Injection: 2µL splitless, Inj.: 210 o C splitter open at 0.75 min. Det.: ECD, 300 o C Sample: 50ug/L in hexane Endrin Aldehyde Methoxychlor SPB-1701 Bleed Advantage Competitor B

15 Alcohol Analysis on a 30m x 0.25mm ID, 0.25µm Column SPB-1701 Competitor B

16 Alcohol Analysis: Elution Order 1. Methanol Pentanol 2. Ethanol Methyl-1-Butanol 3. Acetone (solvent) Methyl-3-Pentanol 4. t-butanol Methyl-1-Butanol 5. n-propanol Methyl-2-Pentanol 6. 1-Methyl-1-Propanol 15. Amyl Alcohol 7. 2-Methyl-1-Propanol Methyl-1-Pentanol 8. n-butanol Hexanol 9. 3-Methyl-2-Butanol

17 Alcohol Analysis: Run Conditions Column: 30m x 0.25mm ID, 0.25µm Oven: 40 o C, (5 min.) 4 o C/min to 100 o C Inj.: 200 o C Det.: FID, 250 o C Flow: 20cm/sec 40 o C Injection: 0.5µL, 100:1 split Sample: 5g/L in acetone

18 Aromatics Analysis on a 30m x 0.25mm ID, 0.25µm Column SPB-1701 Competitor B

19 Aromatics Analysis: Elution Order 1. Hexane (solvent) 8. Cumeme 2. Benzene 9. n-propylbenzene 3. Toluene 10. 1,3,5-Trimethylbenzene 4. Nonane 11. 1,2,4-Trimethylbenzene 5. Ethylbenzene 12. 1,2,3-Trimethylbenzene 6. m/p-xylene 13. n-c10 Aromatic Isomers 7. o-xylene

20 Aromatics Analysis: Run Conditions Column: 30m x 0.25mm ID, 0.25µm Oven: 60 o C, (12 min.) 6 o C/min to 120 o C Inj.: 200 o C Det.: FID, 200 o C Flow: 25cm/sec 60 o C Injection: 0.5µL, 100:1 split Sample: 5g/L in hexane

21 TIC of 8270 Run

22 8270 Run Elution Order 1. 1,4-Dichlorobenzene-d4 10. Benzo(a)Anthracene 2. Bis(2-chloroethylether) 11. Chrysene 3. Aniline 12. Benzo(b)Fluoranthene 4. Phenol 13. Benzo(k)Fluoranthene 5. N-Nitroso-di-n-propylamine 6. Hexachlorocyclopentadiene 7. Acenaphthene-d10 8. Phenanthrene-d10 9. Benzidine

23 8270 Run Conditions Column: 30m x 0.25mm ID, 0.25µm SPB-1701 Oven: 40 o C, 8 o C/min to 280 o C Inj.: 280 o C Det.: MSD, Interface at 280 o C, scan range amu Flow: He, 30cm/sec at 160 o C Injection: 1µL, splitless; splitter open at 0.50 min Sample: 50µg/mL in methylene chloride

24 Mass Spectra of Column Bleed at 280 o C

25 Alditol Acetate Derivatives of Sugars Pentoses Hexoses Amino Sugars

26 Alditol Acetates: Elution Order 1. Rhamnose 8. Galactose 2. Fucose 9. Glucose 3. Ribose 10. Myoinositol 4. Arabinose 11. Muramic Acid 5. Xylose 12. Galactosamine 6. Allose 13. Glucosamine 7. Mannose 14. Methyl Glucamine

27 Alditol Acetates Analysis: Run Conditions Column: 30m x 0.25mm ID, 0.25µm Oven: 220 o C, (2 min.) 10 o C/min to 270 o C Inj.: 250 o C Det.: FID, 280 o C Flow: 30cm/sec 220 o C Injection: 0.5µL, 100:1 split Sample: various concentrations in ethyl acetate

28 Organophosphorous Pesticides on a 30m x 0.25mm ID, 0.25µm SPB

29 Organophosphorous Pesticides (cont.)

30 Organophosphorous Pesticides Column: 30m x 0.25mm ID, 0.25µm SPB-1701 Oven: 50 o C, (hold 1 min.), 25 o C/min to 100 o C (hold 2 min.), 5 o C/min. to 280 o C Inj.: 280 o C Det.: MSD, Interface at 300 o C, scan range amu Flow: He, 35cm/sec at 50 o C Run Conditions Injection: 1µL, splitless; splitter open at 0.50 min Sample: 20µg/mL in hexane

31 Summary New SPB-1701 column has been developed Numerous variations in phase chemistry are used and the phase chemistry affects column selectivity/ polarity SPB-1701 selectivity is similar to the most widely used columns SPB-1701 is the lowest bleed of the 1701 type columns SPB-1701 can be used for a variety of applications