Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange...

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Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 [email protected]

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Transcript of Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange...

Page 1: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Capillary Columns

Nicholas H. Snow

Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ

07079

[email protected]

Page 2: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Capillary/Open Tubular Column

Page 3: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

WCOT - Wall Coated Open Tubular

Page 4: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Capillary Column Dimensions

Page 5: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Other Types of Capillary Columns

Page 6: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Tubing Material

• Stainless Steel– reactive

• Glass– can be made inert– difficult to handle

• Fused Silica– flexible– most inert– most popular

Page 7: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Fused Silica Surface

• Contains 0.1% -OH groups

• Very inert• Uniform chemical

surface

Page 8: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Fused Silica

• High tensile strength• Flexible• Sheath of polyimide• Very inert

Page 9: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Capillary vs. Packed

Page 10: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Packed Column - ECD

Page 11: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Capillary Column - ECD

Page 12: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Important Column Parameters

Page 13: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Column Diameter

Page 14: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Column Length

Page 15: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Column Length Recommendations

Page 16: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Stationary Phase Film Thickness

• Starting point: 0.25m• Compromise: resolution and

capacity• Practical operating

temperatures• Speed or resolution

Page 17: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Thick Film Stationary Phase

• Advantages– increased retention for

volatiles

– increased capacity

• Disadvantages– less efficient

– higher temperatures

– higher bleed

Page 18: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Natural Gas

Page 19: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Thin Film Stationary Phase

• Advantages– high efficiency

– lower elution temperatures

– fast analysis

• Disadvantages– low capacity

– limited trace analysis

Page 20: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Thin Film SeparationAir Freshener

Page 21: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Stationary Phase Requirements

• Selectivity

• Low Bleed Rate

• Reproducibility

Page 22: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Common Stationary Phasespolysiloxane gum phases

Page 23: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Stationary Phasespolyglycol

Page 24: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Crosslinked Stationary Phases

• More stable• Clean by rinsing• Longer lifetimes

Page 25: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Carrier Gas Flow Rate

Page 26: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Review - Capillary Columns

Page 27: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Review - Capillary Columns

Page 28: Capillary Columns Nicholas H. Snow Department of Chemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079 snownich@shu.edu.

Column Selection


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