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GC Instruments: - Fairly Simple Instrumentation

This document discusses gas chromatography (GC) instrumentation. It covers the basic components of a GC system including columns, sample introduction techniques, and detectors. The key points are: - Maintaining constant average pressure is important for GC. Pressure controls flow rate and changing flow rate affects the chromatogram. - The most common sample introduction techniques are direct injection and split/splitless injection. Split/splitless injection is commonly used for capillary columns to avoid overloading. - There are two main types of columns: packed and open tubular (capillary). Capillary columns are more commonly used and have smaller diameters and different stationary phase coating materials than packed columns.

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Chitrakshi Goel
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102 views

GC Instruments: - Fairly Simple Instrumentation

This document discusses gas chromatography (GC) instrumentation. It covers the basic components of a GC system including columns, sample introduction techniques, and detectors. The key points are: - Maintaining constant average pressure is important for GC. Pressure controls flow rate and changing flow rate affects the chromatogram. - The most common sample introduction techniques are direct injection and split/splitless injection. Split/splitless injection is commonly used for capillary columns to avoid overloading. - There are two main types of columns: packed and open tubular (capillary). Capillary columns are more commonly used and have smaller diameters and different stationary phase coating materials than packed columns.

Uploaded by

Chitrakshi Goel
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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GC Instruments
Fairly simple instrumentation

Maintaining constant average pressure is important!


Pressure controls flow rate (T too)

Flow rate monitoring

Changing flow rate changes chromatogram (B/u)


Sometimes use Retention Volume (Vg)

GC Instruments - Sample Introduction


Want small plug
Can doom the separation from the start!

Most common: Direct injection (microflash vaporizer)

Inject and vaporize simultaneously


Need appropriate temperature

Ideally low dead volume Fairly low maintenance

More precise: Injection Loop Headspace and Purge-andTrap methods SPME

GC Instruments - Sample Introduction


Split/Splitless Injection Most common for capillary columns
Avoids overloading

Split ratio is controllable by adjusting carrier gas flow through split vent.

GC Instruments - Columns
Two general classes: Packed and Open Tubular
three components: column, support, coating

Packed Columns
Column materials: glass, metal (stainless), Teflon
few meters in length few mm in diameter (i.d.)

Support Materials:
small particles, uniform (spherical) shape, porous, inert
Typically 100-300 m diameter

Most common: diatomaceous earth


also polymeric materials

Capillary (Open Tubular) Columns


Column materials
Small diameter (typically <500 m) metal, plastic, glass (FRAGILE) More recently: Fused Silica - robust, flexible

Support methods:
Support-Coated OT: Wall-Coated OT

GC Instruments Columns
Stationary Phase Materials
Gas-Liquid Chromatography (GLC) Characteristics:
appropriate chemical nature (like dissolves like) low volatility thermal stability chemical inertness

Typical coatings (< 1 to several m thickness):


Polyethylene Glycol (PEG, Carbowax)

(O
Poly(dialkyl)silane:

CH2 R

CH2 n

(O

Si R

)n

Vary R groups to vary retention characteristics

GC Instruments - Columns
Lifetime of column is limited by:
adhesion of liquid coating to stationary phase (bleeding) irreversible adsorption of contaminants to column

Minimizing bleeding
Cross-linking: on-column reaction Bonding: Utilize surface chemistry of column (or packing)
OH Si O OH Si O OH Si O
catalyst

Si

Si

Si

Minimizing Adsorption
CH3 OH Si

Cl Si Cl
catalyst

Cl CH3 CH3 Si O Si CH3


CH3OH

CH3 CH3 Si O Si CH3

Gas-solid Chromatography (GSC):


Typically porous solid adsorbed to walls (OT) or a porous solid support
molecular sieves Porous polymers (beads or coatings)

GC Instruments - Detectors
Characteristics of a good detector
Sensitivity appropriate to sample Large linear dynamic range Useful at a range of temperatures Rapid response time Easy to use (idiot proof?) Stable, Predictable response Nondestructive (probably least important)

GC Instruments Detectors
Flame Ionization Detector (FID)
Column effluent is passed through a H2-Air flame
Produces ions and electrons

Charged particles are accelerated by voltage applied between jet and collector
results in current (pA)

Number of ions depends on number of reduced (methylene) carbons in molecule


one molecule of ethane gives twice the signal of one molecule of methane less sensitive for non-hydrocarbon groups insensitive to H2O, CO2, SO2 and other noncombustibles

High sensitivity, good LDR (107) , low noise, destructive

GC Instruments - Detectors
Thermal Conductivity Detector (TCD):
Element is electrically heated at constant power
Temperature depends on thermal conductivity of surrounding gas

Measure conductivity (resistance) with respect to a reference Hydrogen and helium carrier gas provide best sensitivity
most thermally conductive Organics are less so when analyte comes off, filament temperature goes up, resistance goes down

Poorer sensitivity than FID, but more universal Large LDR (105), non-destructive

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GC Instruments Detectors
Electron Capture Detector (ECD):
Carrier gas (and analyte) passes over -emitter, resulting in ionization and e- production Produces current between electrodes In the presence of other compounds (especially halogens, etc.) electrons are captured, causing decrease in current Most commonly used for halogenated organics (insecticides, etc.), small LDR (102)

Other Detectors:
Atomic Emission
Microwave induced plasma, grating monochromator, diode array detector

Mass Spectrometry Detection Thermionic Detector


Sensitive to phosphorous and nitrogen

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Quantitative and Qualitative Analysis


Qual.: Retention Index (Kovats Number)
Regardless of column, separation conditions, etc., define the retention index (RI) of a normal alkane as 100n, where n = # of aliphatic carbons RI = 100n RI for all other compounds will vary, depending on experimental conditions, but RI for n-alkanes is fixed. RI is related to retention time!
' (U) log tr' (n) log tr RI = 100 n + (N n) ' ' (n) log tr (N) log t r

Useful for comparing multiple components in a separation

Quant:
To a large degree, sensitivity is controlled by the detector, while selectivity is controlled by the separation conditions Both need to work well to provide good accuracy and precision!

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Two-dimensional GC
Coupled GC columns
Heart-cut or Comprehensive

Leads to improved qualitative (ID) information

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