Objective Introduction Many samples of interest to chemists are complex mixtures of many individual components.

s. Analysis of a particular substance in the mixture is complicated by the presence of other substances. Therefore complex mixtures must often be separated into the individual components prior to analysis. One technique used for separating and analyzing the components of a solution is Gas Chromatography (GC). This technique is useful for gases or volatile compounds that vaporize quickly. It is based on the partition or distribution of the sample components between gaseous mobile phase and liquid phase that is coated on the surface of an inert solid (the GC column). A sample is injected onto the head of a column (see Figure 10.1). The injector and column are heated to a temperature that is high enough to vaporize the sample. A gas such as helium flows through the column; this is the mobile phase or carrier gas and it serves to carry the sample from the injector, through the column and into the stationary phase; the stationary phase selectively interacts with components in the sample and accomplishes the separation. A competition is established between the mobile and stationary phase for the individual compounds passing through the column. The rate at which the sample component passes through the column depends on the degree of interaction between the sample and the column and on the boiling point of the sample. If the component does not interact with the column, it moves through the column, swept by the mobile phase, in a relatively short time. If the component interacts with the column, a longer time is needed for the sample through the column. A components identity can be determined by its retention time. Retention time is the time required for the component to appear at the detector. Components that move through the column quickly have short retention times while components that interact with the stationary phase and linger on the colurrin have longer retention time. In this experiment, the composition of an unknown alcohol mixture is determined by using gas chromatography. To identify the component of an unknown alcohol mixture To determine the composition of an unknown alcohol mixture

Figure 10.1

APPARATUS 1. GC System, Perkin Elmer Auto System XL Gas Chromatograph-Thermal conductivity detector.

2. Column-V4 in (o.d) x 0.5 m Pgropack column.

3. Micro syringe (10L)

CHEMICAL SUPPLIES 1. Methanol 2. Ethanol 3. Isopropanol 4. Unknown mixture of alcohols

CAUTION: Dispose of all organics in the proper waste container. Safety: Handle the syringe carefully. The syringe is very dangerous, especially when filled with hazardous chemicals. They also break easily. Do not allow the syringe to roll off of the lab bench. When injecting the sample, push the plunger straight so that it does not bend. The gas chromatograph is like oven, so the port may be hot. Use caution.

RESULT A. Gas Chromatograph Settings Column Temperature Detector Temperature Injection Port Temperature : : : 100C 130C 120C

B. Chromatograph Data Alcohol Standards Standard Methanol Ethanol Isopropanol Retention Time (min) 2.36 1.53 2.14

Identification of Unknown Mixture Unknown Sample Peak 1 Peak 2 Peak 3 Retention Time (min) 1.58 2.17 Peak Area 1 39262.32 273580.39 Peak Area 2 Average Peak Area -

Percentage Composition of each Alcohol in the Mixture Unknown Sample Peak 1 Peak 2 Percentage Composition (%) 12.55 87.45

The Calculation of Percentage Composition of each Alcohol in the Mixture using the Formula above Percentage X = Peak Area of X x 100 Total peak area of all peaks

DISCUSSION The instrument use to identify the component of an unknown alcohol mixture and determine the composition of an unknown alcohol mixture is Gas Chromatography (GC). GC is widely used method for separation, identification and determination of chemical component in complex mixtures. It is useful for gases or volatile compounds that vaporize quickly. GC is based on the partition or distribution of the sample components between gaseous mobile phase and liquid phase that is coated on the surface of an inert solid (the GC column). The retention time of methanol is 2.36 minutes while for ethanol; the retention time is 1.53 minutes. Then, the retention of isopropanol is 2.14 minutes. So that, the first objective to identify the component of an unknown alcohol mixture was achieved. Then, the composition of an unknown alcohol mixture was determined. The retention time and area for peak 1 is 1.58 minutes and 39262.32 V-s and show the present of ethanol. Then, the retention time and area for peak 2 is 2.17 minutes and 273580.39 V-s and show the present of isopropyl. Ethanol and isopropanol that present in the unknown alcohol mixture while methanol was not. The most probably reason of this result is the unknown sample was contaminate from the syringe used. The syringe must rinse at least 6 times, if not, the compound will contaminated and affect the graph of result. The percentage composition of ethanol is 12.55% while isopropyl is 87.45%. The calculation of percentage composition of each alcohol in the mixture using the formula above Percentage X = Peak Area of X x 100 Total peak area of all peaks

CONCLUSION The instrument use to identify the component of an unknown alcohol mixture and determine the composition of an unknown alcohol mixture is Gas Chromatography (GC). The percentage composition of ethanol is 12.55% while isopropyl is 87.45%. During the experiment, the same syringe was used to inject the standard solution and unknown sample, so that the syringe must rinse at least 6 times to prevent the contamination because it will affect the pattern of graph. Then, the syringe must be handling carefully because it is very dangerous, especially when filled with hazardous chemicals. Besides, it also breaks easily. Do not allow the syringe to roll off of the lab bench. When injecting the sample, push the plunger straight so that it does not bend. Another caution is the GC is like oven, so the port may be hot. The objectives of this experiment were achieved.

APPENDIXES Pre Laboratory Question 1. What is Gas Chromatography (GC)? Gas chromatography (GC) is a powerful method for the separation and analysis of volatile components of mixtures. Like all chromatographic methods, its operation is based on the distribution of the sample components between a mobile phase and a stationary phase. A sample is introduced into a heated injector, carried through a separating column by an inert gas, and detected as a series of peaks on a recorder when components leave the column 2. Explain the separation column in GC? Since the partitioning behavior is dependent on temperature, the separation column is usually contained in a thermostat-controlled oven. Separating components with a wide range of boiling points is accomplished by starting at a low oven temperature and increasing the temperature over time to elude the high-boiling point components. Separation involves the use of a stationary phase and a mobile phase. Components of a mixture carried in the mobile phase are differentially attracted to the stationary phase and thus move through the stationary phase at different rates. The mobile phase is an inert carrier gas and the stationary phase is a solid or liquid coated on a solid contained in a coil column.

Post Laboratory Question 1. Why we need to make sure there is no bubble in syringe during injection of sample into GC. We need to make sure there is no bubble in syringe during injection of sample into GC because it will affect the smooth of graph.

REFERENCE

John W.Lehman, The Student s Lab Companion Laboratory Technique for Organic Chemistry, Pearson Education, Upper Saddle River, New Jersey, 2004, p205