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  2. 2. My summer training in the esteemed K.D.M.I.P.E Dehradun comprised me to possess articulate knowledge about various instrumentation techniques to characterize the organic matter contained in petroleum source rocks, which generate petroleum in a hydrocarbon productive basin.
  3. 3. • The instrumentation techniques described further are important tools for bulk and molecular level characterization of organic matter, which are precursors of petroleum. • The rocks, which contain organic matter, are called petroleum source rocks. • Once, the source rocks get sufficient heat energy they become thermally mature and generate hydrocarbons. • The thermally mature source rocks are called Effective Source rocks. Whereas, the thermally immature rocks are called Potential Source rocks. • These source rocks are studied in a basin wide scale with the help of sophisticated analytical techniques.
  4. 4. Rock Eval Analysis (RE-6) Rock Eval Pyrolysis method has been in use for oil prospecting in Sedimentary Basins all over the world. The previous equipment, Rock Eval-2 and Rock Eval-5 provided data on the quantity and quality of organic matter in sedimentary rocks. The new Rock Eval-6 has been developed to enlarge the field of application of both organic and mineral carbon, a better precision for temperature measurements allow acquisition of data for kinetics and overall higher temperature ranges allow a better characterization of TOC and Tmax.
  5. 5. PYROLYSIS • Pyrolysis is the decomposition of organic matter by heating in the absence of oxygen. • Organic geochemists use pyrolysis to measure the richness and maturity of potential source rocks. • In a pyrolysis, the organic content is pyrolyzed in the absence of oxygen, then combusted. The amount of hydrocarbons and carbon dioxide released is measured. • The most widely used pyrolysis technique is Rock-Eval.
  6. 6. Rock-Eval Pyrolysis • In Rock-Eval pyrolysis, a sample is placed in a vessel and is progressively heated to 550°C under an inert atmosphere. • During the analysis, the hydrocarbons already present in the sample are volatized at a moderate temperature. • The amount of hydrocarbons are measured and recorded as a peak known as S1. • Next pyrolyzed is the kerogens present in the sample, which generates hydrocarbons and hydrocarbon-like compounds (recorded as the S2 peak), CO2, and water. • The CO2 generated is recorded as the S3 peak. • Residual carbon is also measured and is recorded as S4.
  7. 7. Analysis Scheme
  8. 8. Peak Is a measurement of… Comments S1 mg Hc/g rock The free hydrocarbons present in the sample before the analysis These are hydrocarbons which have already been generated and present in rock. S2 mg Hc/g rock The volume of hydrocarbons that formed during thermal pyrolysis of the sample Used to estimate the remaining hydrocarbon generating potential of the sample S3 mg Hc/g rock The CO2 yield during thermal breakdown of kerogen Most prevalent in calcareous source rocks. S4 mg Hc/g rock The residual carbon content of the sample Residual carbon content of sample has little or no potential to generate hydrocarbons due to a lack of hydrogen in the chemical structure of the molecule PYROLYSIS INDICES
  9. 9. AUTOMATIC KEROGENATRON SYSTEM Automatic Kerogenatron System is used for the isolation of the organic matter from a sedimentary sample after destruction of the mineral matrix by acid treatment.
  10. 10. • Automatic Kerogenatron is an instrument used to extract the kerogen from the sedimentary rocks. • Kerogen is the organic part of the rock which is converted to hydrocarbons (oil and gas) on thermal maturation. • The extracted kerogen is studied further on molecular level. By GC (Gas Chromatograph) and GS-MS (Gas Chromatograph and Mass Spectrometer) studies, we come to know about the detailed structure of kerogen.
  11. 11. Procedure • Kerogen is extracted from the rocks by breaking the inorganic part. This is done by the treatment of HF+HCl at temperatures 70-80 degree Celsius. • This acid treatment is done successively three times followed by washing with water. • By successive acid treatment the inorganic part of the rocks like carbonates, phosphates and silicates are broken and washed by water. Thus only organic part that is, kerogen remains after acid treatment. • Kerogen is dried by Nitrogen gas.
  12. 12. Fluorescence Microscope with Image Analysis System
  13. 13. • Flouroscence microscope is used to measure the reflectance of light from the surface of Vitrinite particles. • The reflectance of light is directly proportional to the thermal maturity of rocks. • Vitrinite is an organic part of the rock which comes from woody part of the plants. • The reflectance of light from the Vitrinite particles increases with increase in thermal maturity.
  14. 14. Procedure • Powdered rock sample is taken and mounted on the top of an Epoxy-raisin block. Epoxy-raisin is a semi solid raisin. On keeping this mixture overnight, we find that this mass turns into solid block. • The surface of the block is polished and seen under a fluorescence microscope. • In the microscope, the Vitrinite particles are clearly identified and a beam of light is thrown on the surface of the rock. • The reflected light is measured and the software calculates the % of reflectance. • This science is called is called Organic Petrography.
  15. 15. For instance in case of hard, shiny coal-the thermal maturity is much more compared to soft coal, which is not shiny. Increased thermal maturity leads to greater production of hydrocarbons.
  16. 16. Elemental Analysis
  17. 17. • In elemental analysis, we measure the concentration of CHNSO (Carbon, Hydrogen, Nitrogen, Sulphur and Oxygen) elements in the rocks. • By this we find out the ratio of H/C and O/C. • H/C ratio indicates the amount of hydrogen in kerogen. • O/C ratio indicates the amount of Oxygen in the kerogen. • The amount of Hydrogen is directly proportional to the potential of rocks for generation of hydrocarbons. • The amount of Oxygen is inversely proportional to the potential of rocks for generation of hydrocarbons. • That is the reason that the source rocks deposition at deep sea generates more hydrocarbons because they exist in anoxyic environment.
  18. 18. Procedure • Rock sample is taken in a crucible and heated at 1200 degree Celsius in a flow of oxygen. • Because of high temperature and the flow of oxygen, flash combustion takes place and all the carbon converts into carbon-di-oxide, hydrogen into water, nitrogen into nitrogen- di-oxide and sulphur into sulphur-di-oxide. • The concentration of carbon-di-oxide, water, sulphur-di-oxide and nitrogen-di-oxide is quantitatively measured by TCD technique (Thermal Conductivity Technique) • Now elemental composition of rock that is, CHNS % can be derived.
  20. 20. • This technique is used to find out the Total Organic Carbon, which is the basic parameter to characterize a petroleum source rock. • A minimum of 2% Total Organic Carbon is required for hydrocarbon generation.
  21. 21. Procedure • In this technique, first of all rock is taken and all inorganic carbon is removed by acid treatment. • Then the rock sample is taken in a crucible and introduced into the MULTI EA 2000 ANALYZER. • In MULTI EA 2000 ANALYZER, the rock sample is heated inside a furnace at the temperature 1200-degree-celsius. At this high temperature, all organic carbon gets converted into carbon-di-oxide gas. The concentration of carbon- di-oxide is measured by TDC technique. • By concentration of carbon-di-oxide we can calculate the amount of Total Organic Carbon present in the rock. • More is the Total Organic Carbon, greater is the hydrocarbon generation.
  22. 22. CF-IRMS (CONTINUOUS FLOW-ISOTOPE RATIO MASS SPECTROMETRY) Isotope ratio monitoring on individual components of a mixture, e.g., individual n-alkanes in liquid and gaseous hydrocarbons through a (GC-C-IRMS) under continuous flow conditions is the state of art practice followed internationally.
  23. 23. • The need of on-line sample preparation with rapid analysis has led to the development of a variety of CF-IRMS methods. CF-IRMS (Continuous flow-Isotope ratio mass spectrometry) methodology has brought about significant evolution in sample preparation hardware for the determination of 13C, 15N, 18O, 34S and D of inorganic and organic samples. It was the coupling of capillary gas chromatography (GC) with isotope ratio monitoring mass spectrometer (IRMS) that allowed the dual inlet system to be bypassed and the new arrangement has been widely referred to as “Continuous flow (CF)-IRMS,” because a carrier gas is used during preparation and analysis of samples. • The solid, liquid, or gaseous samples can be analysed on these machines in their natural state, or with minimal sample preparation and process large number of samples per day.
  25. 25. Thank You