Registration no: 19-Arid-1309 Subject: Organic Chemistry Subject code: BCH 302 Group no 7 Analysis of hydrocarbon in common fuels is done by SPME (Solid phase Micro extraction) and Gas chromatography. SPME:
Sample used were petrol, diesel, thinner and
unknown. It is basically a solid phase extraction sampling technique. Solid-phase microextraction, or SPME, is solid phase extraction sampling technique that involves the use of a fiber coated with an extracting phase, that can be a liquid (polymer) or a solid which extracts different kinds of analytes (including both volatile and non-volatile) from different kinds of media, that can be in liquid or gas phase. The quantity of analyte extracted by the fibre is proportional to its concentration in the sample as long as equilibrium is reached or, in case of short time pre-equilibrium, with help of convection or agitation. The advantage of SPME is that the extraction is fast and simple. It can be done usually without solvents, and detection limits can reach parts per trillion (ppt) levels for certain compounds. SPME also has great potential for field applications, on-site sampling can be done even by nonscientists without the need to have gas chromatography-mass spectrometry equipment at each location. When properly stored, samples can be analyzed days later in the laboratory without significant loss of volatiles. After extraction, the SPME fiber is transferred to the injection port of separating instruments, such as a gas chromatography and mass spectrometry where desorption of the analyte takes place and analysis is carried out. The fiber was conditioned in the GC injection port at 2500 degree Celsius for at least 10 minutes to removed contaminants. The sample is added in a glass vial and then vial is placed on a hot plate and sample was heated to 500 degree Celsius while agitate it by using magnetic stirrer. Then the SPME fiber was exposed to the headspace of the vial for 20 minutes. After that the fiber was withdraw into the needle and pulled out from the vial and immediately injected into GC with desorption time 80 seconds. After desorption period, the needle was withdrawn from the injection port and chromatography process continued. After the chromatogram was obtained, the major compounds in each sample were identified using the mass spectra library. For instance, if unleaded petrol was used as sample the results obtained will give the concentration of Toluene, Ethyl benzene and P- Xylene. It is a process of separating components from the given crude drug by using a gaseous mobile phase. It involves a sample being vaporized and injected onto the head of the chromatographic column. The sample is transported through the column by the flow of inert, gaseous mobile phase. The column itself contains a liquid stationary phase which is absorbed onto the surface of an inert solid. Gas-solid chromatography (stationary phase: solid) Gas-liquid chromatography
(stationary phase: immobilized liquid)
Advantages of Gas Chromatography: The technique has strong separation power and even complex mixture can be resolved into constituents. The sensitivity of the method is quite high. It gives good precision and accuracy. The analysis is completed in a short time. The cost of instrument is relatively low and its life is generally long. The technique is relatively suitable for routine analysis.