How can liquids be analyzed with gas chromatography




















It is coiled up so that it will fit into a thermostatically controlled oven. The column is packed with finely ground diatomaceous earth, which is a very porous rock. This is coated with a high boiling liquid - typically a waxy polymer. It is cooler than the injector oven, so that some components of the mixture may condense at the beginning of the column.

In some cases, as you will see below, the column starts off at a low temperature and then is made steadily hotter under computer control as the analysis proceeds. One of three things might happen to a particular molecule in the mixture injected into the column:.

A compound with a boiling point higher than the temperature of the column will obviously tend to condense at the start of the column. The chances are that it will then condense again a little further along the column. Similarly, some molecules may dissolve in the liquid stationary phase Some compounds will be more soluble in the liquid than others. The more soluble ones will spend more of their time absorbed into the stationary phase; the less soluble ones will spend more of their time in the gas.

The process where a substance divides itself between two immiscible solvents because it is more soluble in one than the other is known as partition.

Now, you might reasonably argue that a gas such as helium can't really be described as a "solvent". But the term partition is still used in gas-liquid chromatography. You can say that a substance partitions itself between the liquid stationary phase and the gas. Any molecule in the substance spends some of its time dissolved in the liquid and some of its time carried along with the gas.

The time taken for a particular compound to travel through the column to the detector is known as its retention time. This time is measured from the time at which the sample is injected to the point at which the display shows a maximum peak height for that compound.

Different compounds have different retention times. For a particular compound, the retention time will vary depending on:. For a given sample and column, there isn't much you can do about the boiling points of the compounds or their solubility in the liquid phase - but you do have control over the temperature. The lower the temperature of the column, the better the separation you will get - but it could take a very long time to get the compounds through which are condensing at the beginning of the column!

On the other hand, using a high temperature, everything will pass through the column much more quickly - but less well separated out. If everything passed through in a very short time, there isn't going to be much space between their peaks on the chromatogram. The answer is to start with the column relatively cool, and then gradually and very regularly increase the temperature. At the beginning, compounds which spend most of their time in the gas phase will pass quickly through the column and be detected.

Increasing the temperature a bit will encourage the slightly "stickier" compounds through. Increasing the temperature still more will force the very "sticky" molecules off the stationary phase and through the column.

There are several different types of detector in use. The flame ionisation detector described below is commonly used and is easier to describe and explain than the alternatives. In terms of reaction mechanisms, the burning of an organic compound is very complicated.

During the process, small amounts of ions and electrons are produced in the flame. The presence of these can be detected. The whole detector is enclosed in its own oven which is hotter than the column temperature. The technique of on-column injection, often used with packed columns, is usually not possible with capillary columns.

The injection system, in the capillary gas chromatograph, should fulfil the following two requirements:. The column s in a GC are contained in an oven, the temperature of which is precisely controlled electronically. When discussing the "temperature of the column," an analyst is technically referring to the temperature of the column oven.

The distinction, however, is not important and will not subsequently be made in this article. The rate at which a sample passes through the column is directly proportional to the temperature of the column.

The higher the column temperature, the faster the sample moves through the column. However, the faster a sample moves through the column, the less it interacts with the stationary phase, and the less the analytes are separated.

In general, the column temperature is selected to compromise between the length of the analysis and the level of separation. A method which holds the column at the same temperature for the entire analysis is called "isothermal.

A temperature program allows analytes that elute early in the analysis to separate adequately, while shortening the time it takes for late-eluting analytes to pass through the column. Generally chromatographic data is presented as a graph of detector response y-axis against retention time x-axis. This provides a spectrum of peaks for a sample representing the analytes present in a sample eluting from the column at different times.

Retention time can be used to identify analytes if the method conditions are constant. Also, the pattern of peaks will be constant for a sample under constant conditions and can identify complex mixtures of analytes. In most modern applications however the GC is connected to a mass spectrometer or similar detector that is capable of identifying the analytes represented by the peaks.

The area under a peak is proportional to the amount of analyte present. By calculating the area of the peak using the mathematical function of integration, the concentration of an analyte in the original sample can be determined.

Concentration can be calculated using a calibration curve created by finding the response for a series of concentrations of analyte, or by determining the relative response factor of an analyte.

The relative response factor is the expected ratio of an analyte to an internal standard or external standard and is calculated by findng the response of a known amount of analyte and a constant amount of internal standard a chemical added to the sample at a constant concentration, with a distinct retention time to the analyte.

In most modern GC-MS systems, computer software is used to draw and integrate peaks, and match MS spectra to library spectra.

In general, substances that vaporize below ca. The samples are also required to be salt -free; they should not contain ions. Very minute amounts of a substance can be measured, but it is often required that the sample must be measured in comparison to a sample containing the pure, suspected substance. Various temperature programs can be used to make the readings more meaningful; for example to differentiate between substances that behave similarly during the GC process.

Professionals working with GC analyze the content of a chemical product, for example in assuring the quality of products in the chemical industry; or measuring toxic substances in soil, air or water. GC is very accurate if used properly and can measure picomoles of a substance in a 1 ml liquid sample, or parts-per-billion concentrations in gaseous samples.

In practical courses at colleges, students sometimes get acquainted to the GC by studying the contents of Lavender oil or measuring the ethylene that is secreted by Nicotiana benthamiana plants after artificially injuring their leaves. In a typical experiment, a packed column is used to separate the light gases, which are then detected with a TCD.

The hydrocarbons are separated using a capillary column and detected with an FID. A complication with light gas analyses that include H 2 is that He, which is the most common and most sensitive inert carrier sensitivity is proportional to molecular mass has an almost identical thermal conductivity to hydrogen it is the difference in thermal conductivity between two separate filaments in a Wheatstone Bridge type arrangement that shows when a component has been eluted.

For this reason, dual TCD instruments are used with a separate channel for hydrogen that uses nitrogen as a carrier are common. Argon is often used when analysing gas phase chemistry reactions such as F-T synthesis so that a single carrier gas can be used rather than 2 separate ones. The sensitivity is less but this is a tradeoff for simplicity in the gas supply. Movies, books and TV shows tend to misrepresent the capabilities of gas chromatography and the work done with these instruments.

In the U. In fact, a typical GC analysis takes much more time; sometimes a single sample must be run more than an hour according to the chosen program; and even more time is needed to "heat out" the column so it is free from the first sample and can be used for the next. Equally, several runs are needed to confirm the results of a study - a GC analysis of a single sample may simply yield a result per chance see statistical significance.

Also, GC does not positively identify most samples; and not all substances in a sample will necessarily be detected. All a GC truly tells you is at which relative time a component eluted from the column and that the detector was sensitive to it.

Please confirm that JavaScript is enabled in your browser. Gas chromatography GC is an analytical technique applicable to gas, liquid, and solid samples components that are vaporized by heat. If a mixture of compounds is analyzed using GC system, each compound can be separated and quantified.

When a mixed solution sample is injected into the GC system, the compounds contained in the sample, including the solvent components, are heated and vaporized within the sample injection unit. With GC system, the mobile phase, referred to as the carrier gas, always flows in sequence from the sample injection unit to the column, and then to the detector.

The target components that were vaporized in the sample injection unit are transported by the carrier gas to the column. Once in the column, the mixture of compounds is separated into the various components, and the amount of each compound is then measured by the detector. The detector converts the amount of each compound into an electrical signal, and sends these signals to a data processing unit.

The data obtained enables determination of the compounds contained in the sample, and in what amounts. The configuration of a GC system is very simple.



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