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CCB 2073 ANALYTICAL CHEMISTRY LABORATORY REPORT

Semester May 2013


Experiment 5: GAS CHROMATOGRAPHY SEPARATION OF ALCOHOLS USING GAS CROMATOGRAPHY
Group No: 6 Members:
1) SATHIYA A/L GUNASEGRAN 17347 2) KINOSRAJ A/L KUMARAN 15352 3) MUHAMMAD HAFIZ BIN MOKHTAR KAMIL 15641 4) NUR ASIAH BT MOHD FAUZI 15369 5) AQILAH BT JAZULI 15626

Date of Experiment: 1TH AUGUST, 2013 Report Submission Deadline: 15TH AUGUST, 2013

Department of Chemical Engineering

1.0 INTRODUCTION
A gas chromatography is used mainly for separation of components in a volatile mixture. Chromatography is a powerful separation method that finds applications in all branches of science. It is very useful instrument for both qualitative and quantitative analysis.. Chromatography encompasses a diverse and important group of methods that allow the separation, identification, and determination of closely related components of complex mixtures. In all chromatographic separations, the sample is dissolved in a mobile phase, which in this experiment, gas.

The mobile phase is then forced through an immiscible stationary phase, which is fixed in a place in a column or on a solid phase. The two phases are chosen so that the components of the sample distribute themselves between the mobile and stationary phases to varying degrees. Some components are strongly retained by the stationary phase, move only slowly with the flow of the mobile phase. Therefore, components that are weakly held by the stationary phase travel rapidly. As a consequence of these differences in migration rates, sample components separate into discrete bands, or zones, that can be analyzed qualitatively and quantitatively.

The type of components and its amount in the sample can then be analyzed in the chromatogram produce by the gas chromatography. The time required for the peak to appear, the retention time, can then be used to identify the components. Areas under the peaks can then be used to measure the relative quantities of the components.

2.0 Experimental Procedure

Instructions for the instruments operation are read and understood before the experiment begun. The gas chromatography (GC) is warmed up beforehand. Setting up the Gas Chromatograph 1. The GC and the software are turned on and started. 2. The following conditions are set for sample analysis. Start 40 C. Hold 3 minutes. Ramp 10 C / min until the temperature is 70 C 3. As a precaution, dont get to close to the port because it may be hot. Running Known Alcohols 1. The sample is injected using auto sampling injection and the data collection is started. 2. The run is stopped by pressing the end button on the computer just after the sample peak of a standard returns to baseline. 3. The data is recorded after the peak obtained. Running Unknown Alcohol Mixture 1. An unknown sample is obtained and the number is recorded. 2. The steps above are repeated for the sample. The data collection is run long enough to get all possible peaks. 3. All the data are recorded. 4. Alcohols present are identified by comparison with retention time of known alcohols. 5. To find % of each alcohol in the sample: The peak area in the sample is recorded. The total area is recorded. % alcohol = area under the alcohol peak total area

3.0 Data and Observation A. Setting up the Gas Chromatograph Starting temperature Holding time Ramping rate Final temperature Data collection 5-6 mins duration 40 C 0 min 1C/m3 70C

B. Running Known Alcohols Standards Methanol Ethanol Isopropanol Retention time (min) 3.235 3.35 3.463

C. Running Unknown Alcohol Sample

Unknown Sample Peak 1 Peak 2 Peak 3 Total

Retention Time 3.235 3.35 3.463

Alcohol Methanol Ethanol Isopropanol

Area 1107926.9 2591361.5 152325.4 3851613.6

% 29 67 4 100

4.0 CALCULATION 1. Calculation of total area ( ( ) ): ( ) ( ) ( )

2. Calculation of % alcohol for each peak.

i. Methanol

ii. Ethanol

iii. Isopropanol

5.0 DISCUSSION

There are two principals of chromatography, which is gas chromatography and liquid chromatography. In this experiment, gas chromatography was used to determine the components present in the unknown mixture of alcohol. Before starting the experiment, all the samples of known alcohol and unknown alcohol was readily prepared by the lab technicians. The data collection duration was set 5-6 minutes even though the retention time is only about 3 to 4 minutes. This is to ensure that the complete process of separation of the mixture of alcohols. The difference in the retention time is due to the volatility of the alcohol. Fluid which is more volatile tend to evaporate or vaporize faster than the less volatile liquid. In this case, methanol is more volatile followed by ethanol and isopropanol. Fluid which is more volatile tend to evaporate or vaporize faster than the less volatile liquid. In this case, methanol is more volatile followed by ethanol and isopropanol. The 35 m long column in the GC allows for a clear separation. The possible main errors include contamination of pure samples by foreign substance and improper calibration of the GC. This can be avoided by proper technique and precautions while conducting the experiment.As an example we can take the syringe, which is not clean, will also affect the results by producing two significant peaks. Lastly, the error could be the instrumentation error. If the gas chromatograph is not calibrated properly, the reading of the retention time will be affected and not accurate. This will make the process of identification of component to be very hard.

6.0 Questions.

7.0 Conclusion

In this experiment, the gas chromatograph has been successfully set up with the correct calibration. The retention time standard database has also been obtained by running the known alcohols. Finally, the composition of the unknown sample have been investigated and concluded as comprising of methanol, ethanol and isopropanol through the peaks observed and compared to the database. In addition, the percentage of composition of alcohol has been calculated, where methanol is 29%, ethanol 67%, and isopropanol 4%.