1. INSTRUMENTATION TECHNIQUES IN
EXPLORATION AND PRODUCTION OF
HYDROCARBONS
PROJECT UNDERTAKEN AT KESHAVA DEVA MALAVIYA INSTITUTE
OF PETROLEUM EXPLORATION (K.D.M.I.P.E)
OIL & NATURAL GAS CORPORATION LTD. (O.N.G.C)
DEHRADUN
APURVA SINHA 110203

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. • 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. 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. 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. 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. Analysis Scheme

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. 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. • 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. 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. Fluorescence Microscope with
Image Analysis System

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. 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. 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. Elemental Analysis

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. 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.

19. DETERMINATION OF TOTAL
ORGANIC CARBON (TOC)
BY MULTI EA 2000
ANALYZER

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. 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. 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. • 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.

24. THE PRINCIPLE OF CF-IRMS

25. Thank You