Improved Performance for Cyanopropylphenyldimethylpolysiloxane (SPB-1701, SPB-1301) Capillary Columns L.M. Sidisky, Yizeng Ni, Greg Baney, Rodney George, Katherine K. Stenerson 01-0026 T401044 CFK
Discussion Topics Introduction Phase Chemistry/ Composition Polarity Comparison Bleed Comparison Applications Summary 01-0027
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 01-0028
Typical Phase Composition % Methyl % Phenyl % Cyano Competitor A 88 6 6 Competitor B 88 6 6 Competitor C 87 8 5 Silphenylene 89 7 4 SPB-1701 88 6 6 01-0029
KRI Polarity Comparison Average KRI values for 2-Octanone Competitor A- 1087.9 Competitor B- 1087.6 Competitor C- 1097. 1 Silphenylene- 1089.9 SPB-1701-1087.7 01-0030
Selectivity Difference 30m x 0.25mm ID x 0.25µm Competitor C SPB-1701 01-0031
Discussion Topics Introduction Phase Chemistry/Composition Polarity Comparison Bleed Comparison Applications Summary 01-0032
Competitor A: 30m x 0.25mm ID x 0.25µm Bleed 46 pa at 280 o C 01-0033
Competitor B: 30m x 0.25mm ID x 0.25µm Bleed 280 o C 25 pa 20 pa 67 pa 01-0034
SPB-1701: 30m x 0.25mm ID x 0.25µm Bleed 280 o C 01-0035
Discussion Topics Introduction Phase Chemistry/ Composition Polarity Comparison Bleed Comparison Applications Summary 01-0036
Peak Symmetry on SPB-1701 - 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 1 1 3 3 Better response on later eluting compounds... 6 Increased tailing on competitor column... 6 3 min. 4 min. 5 min. 01-0037
Organochlorine Pesticides on a 30m x 0.53mm ID, 0.50µm Column 01-0039
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 01-0040
Alcohol Analysis on a 30m x 0.25mm ID, 0.25µm Column SPB-1701 Competitor B 01-0043
Alcohol Analysis: Elution Order 1. Methanol 10. 3-Pentanol 2. Ethanol 11. 1-Methyl-1-Butanol 3. Acetone (solvent) 12. 3-Methyl-3-Pentanol 4. t-butanol 13. 2-Methyl-1-Butanol 5. n-propanol 14. 4-Methyl-2-Pentanol 6. 1-Methyl-1-Propanol 15. Amyl Alcohol 7. 2-Methyl-1-Propanol 16. 4-Methyl-1-Pentanol 8. n-butanol 17. 1-Hexanol 9. 3-Methyl-2-Butanol 01-0044
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 He @ 40 o C Injection: 0.5µL, 100:1 split Sample: 5g/L in acetone 01-0045
Aromatics Analysis on a 30m x 0.25mm ID, 0.25µm Column SPB-1701 Competitor B 01-0046
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 01-0047
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 He @ 60 o C Injection: 0.5µL, 100:1 split Sample: 5g/L in hexane 01-0048
TIC of 8270 Run 01-0049
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 01-0050
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 45-450 amu Flow: He, 30cm/sec at 160 o C Injection: 1µL, splitless; splitter open at 0.50 min Sample: 50µg/mL in methylene chloride 01-0051
Mass Spectra of Column Bleed at 280 o C 01-0052
Alditol Acetate Derivatives of Sugars Pentoses Hexoses Amino Sugars 01-0053
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 01-0054
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 He @ 220 o C Injection: 0.5µL, 100:1 split Sample: various concentrations in ethyl acetate 01-0055
Organophosphorous Pesticides on a 30m x 0.25mm ID, 0.25µm SPB-1701 01-0056
Organophosphorous Pesticides (cont.) 01-0057
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 50-500 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 01-0058
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 01-0059