Introduction to Gas Chromatography
Jeffrey Palumbo
ID: 20523300
Chem 224L
Section 003
Partner: Victor Łotocki
Date of Experiment: June 17, 2015
Introduction
Gas chromatography is a common separation technique used in analytical chemistry to separate, identify and quantify the compounds present is a sample (Harris, 2010). The purpose of this experiment is to analyze a sample of TEX (toluene, ethyl benzene, and o-xylene) and identify the peaks from the resulting chromatogram. Another objective is to familiarize students with the instrumentation and theory behind the technique and compare isothermal and temperature-programmed runs.
There are two different injection methods for gas chromatography, split and splitless. Split injections are best used for samples containing high concentrations of analytes. In this injection method, a fraction of the sample is used and the rest is discarded. The complete injection would contain too much analyte, overload the column, and produce inaccurate results. A splitless injection is used for very dilute solutions. Approximately 80% of the sample is applied to the column and the gas is analyzed by slowly raising the temperature of the column to vaporize the solvent at the head of the column. This method cannot be used for isothermal chromatography (Harris, 2010).
Gas chromatography is similar to other chromatography methods in the sense that it has both a stationary and mobile phase. The mobile phase consists of an inert gas,
Answer: Gas chromatography (GC) – utilized by scientists in order to be able to separate the volatile
On a thin chromatography plate, five spots were placed ( as shown in table 2) and the plate was developed using chloroform/methanol. This was later visualized with dragendorff’s reagent under the UV light. All separated components were observed, identified and recorded.
Introduction: The fundamental techniques of organic chemistry lab, commonly known as SIPCAn, include separation, isolation, purification, characterization, and analysis (1). Through SIPCAn, students learn the fundamental techniques of organic chemistry laboratory. Mastering these techniques are necessary in order to perform more complicated experiments and to carry out organic reactions and synthesis. The information gained from SIPCAn included boiling point, melting point, and density can be used to identify unknown compounds. Simple distillation was used to purify a compound by separating it from a
Different procedures were used to isolate benzil from the ether layer and benzoic acid from the aqueous layers. To isolate benzil, anhydrous MgSO4 was added to the flask containing the ether layer solution. MgSO4 removes the remaining water in the ether layer solution. After making sure that enough amount of MgSO4 present in the solution, the ether solution was filtered by using gravity filtration. During filtration, MgSO4 was removed from the solution and the ether solution was collected in 25 ml flask. To separate benzil from the filtered ether solution, the beaker containing the ether solution was heated until the ether evaporated. After letting the beaker to cool to room temperature, the mass of the beaker with the benzil crystals was measured. From the combined mass of the beaker and the benzil crystals and from the predetermined mass of the beaker, the mass of the collected crystals was calculated to be 0.266 gram.
Distillation is a method of separating two volatile chemicals on the basis of their differing boiling points. During this lab, students were given 30 mL of an unknown solution containing two colorless chemicals. Because the chemicals may have had a relatively close boiling point, we had to employ a fractional distillation over a simple distillation. By adding a fractionating column between the boiling flask and the condenser, we were able to separate the liquids more efficiently due to the fact that more volatile liquids tend to push towards the top of the fractionating column, thereby leaving the liquid with the lower boiling point towards the bottom. After obtaining the distillates, we utilized a gas chromatograph in order to analyze the volatile substances in the gas phase and determine their composition percentage of the initial solution. Overall, through this lab we were able to enhance our knowledge on the practical utilization of chemical theories, and thus also demonstrated technical fluency involving the equipment.
The purpose of this lab is to investigate the processes that can be used to separate two volatile liquids in a mixture based on their chemical properties. This is accomplished by fractional distillation, which separates chemicals in a mixture by differentiating them by their boiling points at atmospheric pressure. Specifically in this lab, fractional distillation is used to separate an unknown mixture into its respective pure components. The components are then identified using gas chromatography, which is also telling of the purity of the extracts and success of the procedure. The procedure of this experiment was specified in lecture by Dr. Fjetland and in Gibert and Martin’s student lab manual, Experimental Organic Chemistry: A Miniscale and Microscale Approach, 6th Edition.
Fractional distillation was required to separate the liquids because isopropyl acetate and toluene have similar boiling points. It allows the liquid with the lower boiling point to evaporate and be collected and separated first. The liquid with the higher boiling point can then evaporate and be collected. The purpose of re-distillation is to removed most of the liquid with the lower boiling point and leaving a purer toluene in the vial. The working principle of gas chromatography is that once the solution is
The compound being tested is placed as a liquid into the gas chromatogram and it is vaporized. The mobile phase is a gas, and the vaporized sample is pushed through a coiled column by a carrier gas, which is chosen so that it is unreactive with the sample. The coiled column is also coated by a liquid which serves as the stationary phase. The different components will reach the detector of the chromatograph at different points, depending on their boiling points. Substances with lower boiling points will vaporize faster, and will therefore reach the detector faster than their higher boiling point counterparts.
A measurement of around 0.5 µL, for each compound, was inserted into a gas chromatography in such a way, a syringe holding the compound was pushed down into a column and injection occurred to then start the machine in separating the compound. A computer was right beside it, indicating the graph of multiple peaks and later, after a duration of 4 minutes, a graph was printed out and obtained to then analyze the retention times and percent composition. “The percent composition was found by inserting the following values into the following equation,
This distinct property of compounds exploited by the MS, can be used to identify it. Hence, the GC and MS components together can be used for the identification of compounds whereas a stand-alone GC or MS machine will not. It is extremely unlikely that two different compounds will behave in the same way in both a GC and a MS. Therefore, a mass spectrum along with a characteristic retention time, typically helps identify a compounds with a lower possibility of
Gas chromatography is a method that separates the components of a solution and measuring the relative quantities. The useful technique of gas chromatography is for chemicals that do not decompose at high temperatures and when a very small quantity of sample (micrograms) is available. Gas chromatography uses are limited as the decomposition temperature of components within a mixture and the composition of the column; columns cannot withstand temperatures that are above 250-350 ¬oC.
Petroleum analysis makes special use of columns for gas chromatography, with industries expecting continues development of columns for high analytical performances and efficiency.
approximation of the flavor composition as defined by breath-bybreath measurements and shows higher odorant concentration and
In 1941 Martin and Synge, described the discovery of liquid-liquid partition chromatography and also laid the foundation of Gas liquid chromatography and High performance liquid chromatography. They also introduced the concept of the Height Equivalent to the Theoretical Plate, which has since been adopted as the measure of Chromatographic efficiency.
Chromatography is a separation technique in which the mixture to be separated is dissolved in a solvent and the resulting solution, often called the mobile phase, is then passed through or over another material, the stationary phase. The separation of the original mixture depends on how strongly each component is attracted to the stationary phase. Substances that are attracted strongly to the stationary phase will be retarded and not move alone with the mobile phase. Weakly attracted substances will move more rapidly with the mobile phase.