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Gas chromatography

is a chromatographic technique that can be used to separate volatile organic compounds. A gas chromatograph consists of a flowing mobile phase, an injection port, a separation column containing the stationary phase, and a detector. The organic compounds are separated due to differences in their partitioning behavior between the mobile gas phase and the stationary phase in the column.

(2)

Read Out System (5)

(4) (3)

(1)

schematic diagram of a gas chromatograph

Diagram Block GC
1. 2. 3. 4. 5. Mobile Phase Reservoir Sample Inlet Coloumn Detector Read Out System

Instrumentation
Mobile phases are generally inert gases such as helium, argon, or nitrogen. The injection port consists of a rubber septum through which a syringe needle is inserted to inject the sample. The injection port is maintained at a higher temperture than the boiling point of the sample mixture. Since the partitioning behavior is dependant on temperture, the separation column is usually contained in a thermostatcontrolled oven. Separating components with a wide range of boiling points is accomplished by starting at a low oven temperture and increasing the temperture over time to elute the high-boiling point components. Most columns contain a liquid stationary phase on a solid support.

1. Reservoir Mobile Phase / Carrier Gas


Carrier gas The carrier gas must be chemically inert. Commonly used gases include nitrogen, helium, argon, and carbon dioxide. The choice of carrier gas is often dependant upon the type of detector which is used. The carrier gas system also contains a molecular sieve to remove water and other impurities.

2. Sample Inlet
Sample injection port For optimum column efficiency, the sample should not be too large, and should be introduced onto the column as a "plug" of vapour - slow injection of large samples causes band broadening and loss of resolution. The most common injection method is where a microsyringe is used to inject sample through a rubber septum into a flash vapouriser port at the head of the column. The temperature of the sample port is usually about 50C higher than the boiling point of the least volatile component of the sample. For packed columns, sample size ranges from tenths of a microliter up to 20 microliters. Capillary columns, on the other hand, need much less sample, typically around 10-3 mL. For capillary GC, split/splitless injection is used. Have a look at this diagram of a split/splitless injector;

3. Coloumn / Stationary Phase


There are two general types of column, packed and capillary (also known as open tubular). Packed columns contain a finely divided, inert, solid support material (commonly based on diatomaceous earth) coated with liquid stationary phase. Most packed columns are 1.5 - 10m in length and have an internal diameter of 2 4 mm. Capillary columns have an internal diameter < 1 millimeter. They can be one of two types; wall-coated open tubular (WCOT) or support-coated open tubular (SCOT). WCOT columns consist of a capillary tube whose walls are coated with liquid stationary phase. SCOT columns, the inner wall of the capillary is lined with a thin layer of support material such as diatomaceous earth, onto which the stationary phase has been adsorbed. Both types of capillary column are more efficient than packed columns.

Gas chromatography columns are of two designs: Packed columns are typically a glass or stainless steel coil (typically 1-5 m total length and 5 mm inner diameter) that is filled with the stationary phase, or a packing coated with the stationary phase. Capillary columns are a thin fused-silica (purified silicate glass) capillary (typically 10-100 m in length and 250 m inner diameter) that has the stationary phase coated on the inner surface. Capillary columns provide much higher separation efficiency than packed columns but are more easily overloaded by too much sample.

After the components of a mixture are separated using gas chromatography, they must be detected as they exit the GC column. The links listed below provide the details of some specific GC detectors. The thermal-conductivity (TCD) and flame-ionization (FID) detectors are the two most common detectors on commercial gas chromatographs. The requirements of a GC detector depends on the separation application. For example, one analysis might require a detector that is selective for chlorinecontaining molecules, another analysis might require a detector that is non-destructive so that the analyte can be recovered for further spectroscopic analysis.

DETECTOR
Classify with respect to:

Selectivity
Mass Flow versus Concentration based response Linear Dynamic Range Detection limit Destructive?

Detectors
There are many detectors which can be used in gas chromatography. Different detectors will give different types of selectivity. A non-selective detector responds to all compounds except the carrier gas, a selective detector responds to a range of compounds with a common physical or chemical property and a specific detector responds to a single chemical compound. Detectors can also be grouped into concentration dependant detectors and mass flow dependant detectors. The signal from a concentration dependant detector is related to the concentration of solute in the detector, and does not usually destroy the sample Dilution of with make-up gas will lower the detectors response. Mass flow dependant detectors usually destroy the sample, and the signal is related to the rate at which solute molecules enter the detector. The response of a mass flow dependant detector is unaffected by make-up gas

Gas chromatography detectors


GC detectors identify solutes as they exit the chromatographic column. As solutes are eluted from the gas chromatography column they interact with the detector. The GC detector converts this interaction into an electrical signal that is sent to the data system. The magnitude of the signal is plotted versus time (from the time of injection) and a chromatogram is generated. GC detectors use one of several technology types to identify solutes as they exit the column. These methods include thermal conductivity, flame ionization, atomic emission, electron capture, photoionization, flame photometric, chemiluminescence spectroscopy, and nitrogen phosphorous.

Detector Flame ionization (FID) Thermal conductivity (TCD) Electron capture (ECD) Nitrogenphosphorus

Type

Support gases

Selectivity

Dete ctabi lity 100 pg

Dyna mic range 107

Mass flow

Hydrogen and air

Most organic cpds.

Conc entrat Reference ion Conc entrat Make-up ion Mass flow Hydrogen and air

Universal

1 ng

107

Halides, nitrates, nitriles, peroxides, anhydrides, organometallics Nitrogen, phosphorus

50 fg 10 pg

105

106

Flame photometric (FPD)


Photoionization (PID) Hall electrolytic conductivity

Mass flow

Hydrogen and air possibly oxygen

Sulphur, phosphorus, tin, boron, arsenic, germanium, selenium, chromium


Aliphatics, aromatics, ketones, esters, aldehydes, amines, heterocyclics, organosulphurs, some organometallics Halide, nitrogen, nitrosamine, sulphur

100 pg

103

Conc entrat Make-up ion Mass flow Hydrogen, oxygen

2 pg

107

5. Read Out System

4. Detector

FID TCD FPD ECD etc

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