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This report is intended to review the use of materials, apparatus, and analysis machines to do analyses on the source rock sample. To carry out the analyses until the final conclusion is made, they involve the preparations of rock samples, the methodologies to conduct the lab, and the interpretation of analyses results. In this report, every lab works will be discussed part by part, from preparation of sample to the expected result and interpretation.
Soxhlet Extraction
The objective of this lab is to extract the bitumen from the source rock. Material: Source rock sample, copper granule, Ageothropic solvent (93% Dichloromethane, 7% Methanol), and anti-bumping granules Apparatus: Soxhlet extractor, grinder, 180 micron size sieve, cellulose thimble, and rotary evaporator Methodology: 1. The source rock sample is crushed into powder form using grinder. 2. The powder is sieved using 180 micron size sieve. 3. This powder is placed inside the cellulose thimble and loaded into the main chamber of the Soxhlet extractor. 4. Soxhlet extractor comprises of 3 main parts: the flask; the Soxhlet main chamber with distillation arm, cellulose thimble and siphon; the condenser. 5. The flask is filled with Ageothropic solvent with volume 3 to 4 times the volume of the Soxhlet chamber, copper granule, and anti-bumping granules.
Boon Ee Juan 6. The flask with its solvent is heated to reflux. The copper granule is used to absorb sulphur while the anti-bumping granules are used to maintain the boiling of solvent at 100 oC. 7. The solvent vapour travels up the distillation arm and condensed by the cooling circulating water. After that, the warm solvent will drip into the cellulose thimble housing the powder. The bitumen will then dissolve into the warm solvent, leaving non soluble content in the thimble. When the Soxhlet chamber is almost full, the solvent is emptied by flowing through the siphon side arm back into the flask. 8. This cycle will be repeated for 3 days to extract the bitumen from the powdered sample. 9. Rotary evaporator is used to remove the solvent from the final mixture in the flask, yielding the extracted bitumen. 10. The extracted bitumen will be further chromatography into aliphatic and aromatic compound.
Boon Ee Juan The process of mobilising the aliphatic and aromatic compounds through the stationary phase is depending on their polarity. Lets say we want to mobilise the aliphatic compound through the stationary phase, we have to choose petroleum spirit as an eluent that has the approximately same polarity with the aliphatic compound. Since the aromatic compound has higher polarity compared to the aliphatic compound, it will not be mobilised as fast as aliphatic compound. The concept is we mobilise the lesser polarity compound first, then the higher polarity compound using higher polarity eluent solvent. LCC is a good separator of aliphatic and aromatic compounds but it takes longer time to separate them compared to Thin Layer Chromatography (TLC).
Boon Ee Juan 9. The petroleum spirit which is the eluent will move up the TLC plate by capillary action. When the petroleum spirit meet the row of bitumen spots, it will carry along the less polarised aliphatic up the TLC plate. The more polarised aromatic compound will be in stationary phase but they would move very slowly upward. Thus, there is a separation of less polarised aliphatic band on the top and more polarised aromatic at the lower TLC plate. 10. Under the UV light, the band of aliphatic and aromatic compound can be seen. 11. The aliphatic band is scrapped into a flask and mixed with petroleum spirit. 12. The aliphatic compound is then extracted from the mixture. 13. The aromatic band is scrapped into a flask and mixed with dichloromethane. 14. The aromatic compound is then extracted from the mixture.
Boon Ee Juan as mobile phase to transport the vaporized component compounds through the capillary column. The wall of the capillary column is coated with different stationary phase. When the vaporized component compounds or gas stream flow through the capillary column, they will interact with the stationary phase on the wall of the column. Different component compounds interact differently with different stationary phase based on the strength of absorption and in this process, they are separated. Thus, various component compounds will elute at a different time and this is known as the retention time that can be qualitatively used to recognise the component compounds. The exit of the gas stream is monitored by a detector where the retention time and the quantity of the component compounds can be determined. The most commonly used detector is the flame ionization detector (FID) and the thermal conductivity detector (TCD). GC can provide a result call gas chromatogram. The Y-axis shows the intensity whereas the Xaxis shows the retention time of the component compounds. Each peaks show different component compounds eluting at different time with different intensity. The processes are repeated again for extracted liquid aromatic compound.
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Methodology of Mass Spectrometer (MS): 1. Straight after the ejection of component compounds from GC, they are re-injected into the vacuum chamber of MS where they are impacted with electron beam. 2. The electron beam ionized the component compounds and breaking them into ionized molecule fragments with mass to charge ratio m/z. This m/z is the characteristic of the molecule fragments. If the charge is fixed, then the m/z could be represented by the mass. 3. The quadrupole mass spectrometer is the detector of the m/z. It functions using 2 pairs of electrically charged poles that will drive and focus the ionized molecular fragments into the detector. 4. Since the charge of the ionized molecule fragments are fixed, the mass of them would affect the different in their acceleration and momentum when driven by the quadrapoles electric field. Thus, their mass spectra could be obtained.
Boon Ee Juan 5. MS can provide a result call mass spectra. The Y-axis shows the intensity whereas the X-axis shows the m/z ratio. Each peaks show different molecular fragments with different mass. A series of spectrum would be obtained for each separated component compounds in the aromatic and aliphatic after the GC.
Vitrinite Reflectance
The objective of this lab is to use the Vitrinite Reflectance (Vro) to measure the thermal maturity of source rock. The source rock can be an organic rich shale or coal. The present of macerals in the organic rich source rock such as Liptinite, Vitrinite and Inertinite can all be used to measure the thermal maturity of source rock by measuring their reflectance under the photometer microscope but Vitrinite is normally been used. This is because Vitrinite is not strongly prone to oil and gas formation. It is common as a residue in source rocks which spans from a wide range of depth and temperature. It is always present and not drastically reduces because of its oil and gas generation. Thus, it can be found within the whole range of maturity of source rock and using its different reflectance in different maturity to indicate the maturity. Like Liptinite which is oil prone, will generate oil in oil window and then drastically reduce in quantity after it is approaching to the end of oil window. Thus, the maturity of the source rock after that cannot be determined because the liptinite is very less or nearly disappear after the maturity of generating oil. In this case, Vitrinite presence is quite constant. Inertinite is seldom been used because it is present in post-maturity source rock which we are not interested. The review of Vitrinite evolution and changing of reflectance As the source rock is being buried deeper and deeper, the temperature is higher and higher and the time where the kerogen splits into its four distinctive types is called Carbonization Jump. At here, the organic compounds undergo reordering and become aligned parallel to the bedding. The Vitrinite has become dense Vitrinite. The source rock is continuing being buried deeper and temperature increases. The chemical composition of the Vitrinite will correspondingly alter, increasing the reflectivity of Vitrinite. Therefore, the percentage reflection of a beam of normal incident white light from the surface of a polished Vitrinite is a function of the maturity of the maceral and source rock.Thus, at different depth and temperature, the Vitrinite reflectance is different and from the Vitrinite
Boon Ee Juan reflectance, the maturity is measured. The vitrinite reflectance value, Vro for oil window is 0.5; Vro for gas window is 1.2. Comparison Kerogen types are determined by the Von Krevelin graph or hydrogen index (HI) against oxygen index (OI) graph which both the indexes can be measured using Rock Eval. Without using Rock Eval, we can also predict the kerogen types by looking at the macerals in the source rock. The presence of liptinite which is oil prone is corresponding to the kerogen type I and II; Vitrinite which is oil and gas prone is corresponding to the kerogen type III; Inertinite which is non-hydrocarbon producing is corresponding to the kerogen type IV. Material: Source rock, resin, and hardener Apparatus: Grinder, sieve, polish machine, and photometer microscope Methodology: 1. The source rock is crushed into fine powder using grinder and then sieved. 2. The powdered source rock will then be mounted into a cylinder shape by using resin and hardener. 3. This resin block is grounded and polished to a high standard. Poor polishing will lead to spurious reflection measurements. 4. The photometer microscope is calibrated using sapphire or garnet. 5. The polished resin block is then inspected under the photometer microscope to measure the Vitrinite reflectance. Normally 30 to 100 vitrinite measurements are taken. 6. The vitrinite reflectance value, Vro can be used to find the depth of oil and gas windows, igneous intrusion, unconformity and structural deformation such as fault. All these can be found using the Log Vro against depth graph.
Boon Ee Juan 4. A calibration for carbon dioxide, CO2 and moisture, H2O is done with corresponding standards using mixture of calcite and gypsum. 5. Then, the loaded quartz boat is inserted into the combustion tube. 6. The furnace control system can control the temperature to be stepped and subjected to ramping. Since various sources of carbon oxidize, decompose or turn into volatiles in different temperature, the temperature profile is completely programmable into 10 different phases. Just set the starting temperature, end temperature, ramping rate and the amount of time to hold at the ending temperature for each of the phases selected. 7. For analysing TOC, the source rock is normally heated from 350oC to 950oC. (This machine can heat up to 2000oC.) 8. The source rock is combusted using oxygen. Its organic compound and hydrocarbons content are cracked and oxidized to release carbon dioxide, CO2 and moisture, H2O. The CO2 and H2O are then measures using Infrared absorption cells detector. The presence of organic carbon may be verified by finding coincident peaks in H2O and CO2. 9. After that, the source rock is ignited in an inert N2 atmosphere with the afterburner and oxidation catalysts at 120oC. In here, only moisture and carbonate will be detected but not the organic carbon. 10. The result is printed out showing the TOC, moisture and carbonate value. 11. When the analysis is completed, the source rock is removed from the combustion tube.
Rock-Eval Pyrolyzer
The objective of this lab is to identify the potential source rock by using the S1, S2 and S3 peak of the Rock Eval analysis. The Rock-Eval Pyrolyzer is actually running a test to determine the bitumen or hydrocarbon that is readily present in the source rock (S1); cracking the kerogen in the source rock to produce hydrocarbon (S2); carbon dioxide, CO2 in (S3) is used to calculate the amount of oxygen readily present in the source rock. The hydrocarbon index (HI), oxygen index (OI) and production index (PI) can be calculated using S1, S2, S3 and TOC. These indexes will then be used to identify the kerogen type in the source rock. Material: Grain size source rock Apparatus: Weight balance Methodology: 1. 2. 3. 4. 5. 6. The source rock is crushed into small grain size. 60mg of the crushed source rock is weighed using weight balance. The crushed source rock is inserted into the Rock-Eval Pyrolyzer. The crushed source rock is heated in the inert atmosphere with helium. The pyrolysis oven heated and kept isothermally at 300C for 3 minutes. The free hydrocarbons are volatilized, detected by flame ionization detector (FID) and measured as the S1 peak.
Boon Ee Juan 7. The temperature is then increased from 300 to 600C at the rate of 25C/min. This is the phase of volatilization of the very heavy hydrocarbons compounds (>C40) as well as the cracking of nonvolatile organic matter. The hydrocarbons released from this thermal cracking are measured as the S2 peak by flame ionization detector (FID). The temperature at which S2 reaches its maximum depends on the nature and maturity of the kerogen and is called Tmax. 8. The CO2 escaped from the kerogen cracking is trapped in the 300-390C range. This trap is heated and the CO2 is released and detected by thermal conductivity detector (TCD) as S3 peak during the cooling of the pyrolysis oven. 9. The S1, S2 and S3 result is printed out. 10. If S1 is lower and S2 is higher peak, this indicate the rock sample is not yet thermally mature enough to produce hydrocarbon but has the potential to be a source rock. 11. The hydrocarbon index (HI),
3. Kerogen types are determined by the Von Krevelin graph or hydrogen index (HI) against oxygen index (OI) graph.