5.

2 Advanced Formation Evaluation

Core Laboratory Measurements

by Alain Brie

November 2012
Core Measurements

§ Basic Measurements § Special Measurements

– Porosity – Relative Permeability
– Grain Density – Residual Hydrocarbon Saturation
– CEC – Mercury Injection
– SEM, Backscatter Analysis
– Permeability
– X-Ray Diffraction XRD
– Thin Sections
– m & n Archie’s Law Parameters

§ Rock Mechanics
– Elastic Constants
– Rock Strength
– Failure angle
– Thick Walled Cylinders
1 © Alain Brie 2012 Advanced Formation Evaluation
 Laboratory Core Measurements

Sample Preparation
Cleaning
Porosity &
Drying
Permeability HPMI

2 © Alain Brie 2012 Advanced Formation Evaluation

Porosity Measurement on Cores

On a core plug, we measure two of the three volumes:

• Vb Bulk volume
• Vg Grain volume
• Vp Pore volume.
We get the third volume from: Vb = Vg + Vp

Then porosity is obtained as φ = Vp / Vb

3 © Alain Brie 2012 Advanced Formation Evaluation

Bulk Volume Measurement

Volumetric Displacement Method

§ Submerge core, observe volume change
§ Prevent liquid from entering pore space of sample
§ Coat with paraffin (1950-1980)
§ Pre-saturate with liquid (Russian method)
§ Use mercury as test liquid (current method – 1980)

4 © Alain Brie 2012 Advanced Formation Evaluation

4
Bulk Volume

Direct measurement of sample with d

a caliper:
π d2
• Smooth right cylinder Vb = h
h 4
• Vuggy sample
• Full-diameter core

The displaced volume of mercury is

Archimedes’ method in mercury: equal to the volume of the core plug.
• Smooth right cylinder
• Imperfect cylinder
• Rough sample

5 © Alain Brie 2012 Advanced Formation Evaluation

Grain Volume (Boyle’s Law)
P1 P2
PV = nRT
Chamber 1 Chamber 2

Initial Conditions: V1 V2
Vg Valve Valve
n1 = P1 (V1- Vg) / RT closed closed

n2 = P2 V2 / RT
P3 P3

Chamber 1 Chamber 2
V1 V2

Final Conditions: Vg Valve Valve

open closed

n1 + n2 = P3 (V1- Vg+ V2) / RT

P1 (V1 - Vg ) + P2 V2 = P3 (V1 + V2 - Vg) φ = (Vb - Vg) / Vb
6 © Alain Brie 2012 Advanced Formation Evaluation
Pore Volume (Boyle’s Law)

Initial Conditions: P2 (V1 + Vp), P1 Vr

Final Conditions: P3 (Vr + V1 + Vp) = P1Vr + P2 (V1 + Vp)
φ = Vp / Vb
7 © Alain Brie 2012 CoreLab
Advanced document
Formation Evaluation
Bulk Volume Measurement

Archimedes Method
§ Measures mass of core sample,
§ Measure change in weight of core sample submerged in test liquid,
§ Measure change in weight of container and test liquid when sample is
introduced,
§ Must prevent liquid from entering pore space.

8 © Alain Brie 2012 Advanced Formation Evaluation

8
Core-Log Integration – Basic Issues

§ Depth Match
– Adjust cores depths to match logs depths
§ Porosity Type
– Is porosity total or effective?
§ Confining Stress Sensitivity
– Correct data to reservoir Net Mean Stress
– Mean stress depends on
§ Pore pressure
§ Confining (overburden) pressure
§ Temperature
– Confining stress mainly affects:
§ Unconsolidated sandstones
§ Lithologies with natural fracturing or micro-fracturing

9 © Alain Brie 2012 Advanced Formation Evaluation

9
Porosity Variation With Confining Pressure

50

40
Sandstones
Porosity, %

30

20
Shales
10

0
0 1,000 2,000 3,000 4,000 5,000 6,000
Confining pressure, psi

10 © Alain Brie 2012 Advanced Formation Evaluation

10
Sample Preparation - Drying

Core porosity depends on: Shaly sands

§ Cleaning method,
Core Permeability vs. Core Porosity:
§ Drying method, Oven-Dried
Reservoir vs. Humidity-Dried
Compartments & Flow Units
§ Sample quality, 10000.0

§ Sample size,
1000.0
§ Measurement type,

Permeability (md)
100.0

Also consider:
Total vs. Effective Porosity. 10.0

1.0
Humidity-Dried

Oven-Dried

Typically 85-90% + of all RCA Porosity 0.1

0 10 20 30 40
Measurements are good to excellent quality Porosity (%)

11 © Alain Brie 2012 Advanced Formation Evaluation

11
 Porosity in Shaly Sands

S andstone
b
xV
R
M
T
Oy V a r i o uPorosity
kco s T e c hMeasured
niques
irat vo et na - lDPr ioe rd oC so ri et A
y n- aN
Dl e
y suni ts rPi oot ryn oLs oi t gy

12 © Alain Brie 2012 Advanced Formation Evaluation

12
 Whole Core Method

Full Diameter

Heterogeneous

Whole Core
Heterogeneous

§ Use selected pieces from the full or whole core,

– Core sizes 2 ½ to 5 ½ inches in diameter,
– Several inches to several feet long,
§ Most applicable method for very heterogeneous formations, however
this measures vertical permeability.
§ Additional expense limits the number of tests.

13 © Alain Brie 2012 Advanced Formation Evaluation

 Perm Plug Method

1” or 1 1/2”

Plug

Most Common Slab Taken for:

Photography
Description
Archival
§ Most commonly applied method,
§ Uses small cylinder core samples
– ¾ inch diameter
– 1 to a few inches long
§ May not apply to heterogeneous formations unless samples are taken to
represent all rock types.

14 © Alain Brie 2012 Advanced Formation Evaluation

 Permeability Sample Plug Selection

I IIa IIb
Unacceptable
kH
~1 ft ?
Or
Full-
kH Diameter
Suitable
kV kV
III IV V

kV
Full
Diameter
kH Matrix
Only
`4” - 9”

Fracture
k and φ?
Whole Core
Analysis
(2-3 ft)

15 © Alain Brie 2012 Advanced Formation Evaluation

 Lab Procedure for Measuring Permeability

§ Cut core plug from whole core or use sample from whole core,
§ Clean core and extract reservoir fluids, then dry the core,
§ Flow a Fluid through core at several flow rates,
§ Record inlet and outlet pressures for each rate.

16 © Alain Brie 2012 Advanced Formation Evaluation

 Gas Permeability – Steady State
P upstream P downstream

Sleeve Pressure

To Vacuum

Pressure Regulator Calibrated Orifice

q k p1 − p 2
= ⋅
A µ L

17 © Alain Brie 2012 CoreLab

Advanced document
Formation Evaluation
 Gas Permeability – Unsteady State

110

90
Pressure (psig)

70

50

30

10
0 10 20 30 40 50
Time (seconds)

Gas pressure decreases exponentially vs. time. The

decay time constant is A function of plug
permeability.

18 © Alain Brie 2012 CoreLab

Advanced document
Formation Evaluation
 Gas Permeability vs. Liquid Permeability

Gas Flow Liquid Flow

Gas molecules flow at a uniform rate through small pores.

Liquid molecules in the center of the pore move faster than the molecules near the
pore wall.
Measured gas permeability is a function of mean pressure during the measurement.
This effect is called “gas slippage” or “Klinkenberg effect,” after the scientist of first
observed it.

19 © Alain Brie 2012 Advanced Formation Evaluation

 Klinkenberg Correction

1
K A = K∞ + b
Permeability

PMean Permeability is measured at

KA4 Helium
several pressures.
KA3 Air
KA2 Extrapolation to infinite
KA1 Slope
Slope == bb pressure gives liquid
permeability.
Non-reactive liquid
K8
Slippage-corrected
Klinkenberg permeability

0 1
PMean

20 © Alain Brie 2012 Advanced Formation Evaluation

 Klinkenberg Correction

Ka Kl % Difference
10,000 10,000 0 The “Klinkenberg correction,” to
1,000 950 5
convert gas permeability to an
100 90 10
equivalent liquid value, varies with
10 8.0 20
permeability.
1 0.70 30 Low-permeability formations require
0.1 0.06 40 large corrections.
0.01 0.005 50

21 © Alain Brie 2012 After CoreLab

Advanced Formation Evaluation
 Permeability Variation With Confining Pressure

22 © Alain Brie 2012 Advanced Formation Evaluation

 Fluid-Rock Interactions

Fluid-rock interactions affect measurement of permeability

§ Fresh water may cause clay swelling, reducing permeability,
§ Tests may cause fine migration, plugging pore throats and reducing
permeability,
§ Reservoir or synthetic reservoir fluids are generally preferred.

23 © Alain Brie 2012 Advanced Formation Evaluation

 Effect of Core Heterogeneities

Core heterogeneities affect measurements of permeability

§ Naturally fractured reservoirs
– Core plugs represent matrix permeability,
– Total system permeability is higher (matrix + fractures)
§ Core mineralogy problems (salt, gypsum)
§ Human intervention
– Plugging of vugs,
– Sampling bias.

24 © Alain Brie 2012 Advanced Formation Evaluation

Core-Log Integration

Porosity Permeability
Data Porosity Data Data A series of closely spaced
cores measurements is
necessary to tie in depth
with the log data.
Porosity and GR data are
good for that purpose.

25 © Alain Brie 2012 Advanced Formation Evaluation

25
25
 CEC Measurement

-
§ Cation Exchange Capacity measures the fraction of
H+ - NH4+
- - NH4+ exchangeable cations in the rock: Ca, Mg, K, Na,
- Al3+ + 1N NH4Cl - NH4+
Clay -- Ca2+ Clay -- NH4+ that relates to the negative charges on surface per
NH4+
- - NH4+
unit weight.
- K+ - NH4+

Rinse with Ethanol § Two equivalent units of measure:

Ca2+ ,Mg2+, H+, Al3+, K+ – milli-equivalent of hydrogen per 100g (meq+/100g)
– centimol per kg (cmol+/kg) of dry rock
§ The usual measurement method by wet chemistry
- NH4+ - H+
- NH4+
+ 0.1N HCl
- H+ technique is replacement with ammonium acetate
- NH4+ - H+
Clay -- NH4+
NH4+
Clay -- H+
H+ or barium and titration with HCl.
- NH4+ - H+
- NH4+ - H+ § Another technique is the silver-thiourea method of
Measure with centrifugal extraction.
ammonium analyzer
+ x NH4+

26 © Alain Brie 2012 Advanced Formation Evaluation

 X-Ray Diffraction

§ All crystalline materials reflect X-rays from atomic

Quartz
planes within the crystal that yield a unique diffraction
pattern,
Silver Substrate § This allows identification of minerals, including those too
small to be identified by thin section studies.
Illite Chlorite
Mica Kaolinite § For best results clay size particles should be separated
from sand and coarser grain particles.

Mixed
Layer

XRD Spectrum

27 © Alain Brie 2012 Advanced Formation Evaluation

 SEM Analysis

§ Scanning electron microscope provides high

magnification, up to 100,000 times, and large depth of
field images of rock crack sections.
§ The images give nearly a 3D view of the grains and
pore structure in the rock.
§ The X-ray backscatter analysis or EDS (energy
dispersive X-ray spectrometer), also yields elemental
analysis of specific locations for mineral identification.

EDS Spectrum

28 © Alain Brie 2012 Advanced Formation Evaluation

 Mercury Injection Principle

§ Injection pressure depends

on pore throat radius
2 . K .σ . cos θ
r=
Pc
– K = 0.145
– Pc Capillary pressure psi
– σ Interfacial tension 480
dynes/cm
– θ Contact angle 140°
§ Saturation as a function of
injection pressure gives the
distribution of pore sizes.

29 © Alain Brie 2012 Advanced Formation Evaluation

 Mercury Injection Correlation With Permeability

§ P-P: Permeability data (Log) vs Porosity data (Lin)

§ 800 psi data from cores or from logs or from both
§ Winland: Lines of Constant PTR (Pore Throat Radius)
– PTR: estimated using Winland’s R35 equation
§ Uses Pc at 35% Hg saturation to compute predominant PTR
§ Assumes input data was obtained at standard conditions
§ Rocks with same hydraulic characteristics are grouped
– Whichever their lithology or depth or geologic age
– Having similar Pc curves, they have the same rock quality

30 © Alain Brie 2012 Advanced Formation Evaluation

Mercury Injection Correlation With Permeability
0.01

Effective Pore Throat Radius

35% Saturation

Effective Pore Throat Radius (microns)

0.10
R35
12379' K(a)=2.5md
Phi=16%
12525' K(a)=30.5md
Phi=18.5%
12591' K(a)=62.5md 1.00
Phi=19.3%
14208' K(a)=95md
Phi=19.1%
10033' K(a)=192md
Phi=23.5% 10.00
9993' K(a)=516md
Phi=25.5%

100.00
100 80 60 40 20 0

Mercury Saturation
Winland Equation:
Log ( R35 ) = . 732 + . 588 ⋅ Log ( k ) − .864 ⋅ Log (φ )

31 © Alain Brie 2012 Advanced Formation Evaluation

 Capillary Pressure Curves

several Pc values
§ Capillary pressure curves are measured with the
restored state capillary pressure cell or permeable
plate technique.
Non-wetting fluid § The sample impregnated with the wetting fluid,
usually water, is placed in the cell on top of a
Sample saturated saturated porous permeable plate.
100% initially
§ The non-wetting fluid is pushed in at several
pressure values Pc and displaces the wetting fluid
in the sample. Saturation as a function of pressure
yields the capillary pressure curve.
Displaced fluid
from core through
permeable plate

32 © Alain Brie 2012 Advanced Formation Evaluation

 Absolute And Relative Permeabilities

§ Permeability is a medium property and characterizes the capacity to

transmit fluid.
§ When medium is fully saturated with one fluid, the permeability
measurement is said absolute or specific,
§ Relative permeability is the ratio of the effective permeability to a fluid
at a given saturation to the absolute permeability of the wetting
phase.

33 © Alain Brie 2012 Advanced Formation Evaluation

 Oil-Water Relative Permeability

34 © Alain Brie 2012 Advanced Formation Evaluation

 Effect Of Wetability

35 © Alain Brie 2012 Advanced Formation Evaluation

 Reservoir Rock Characterization From Cores

§ Relate deposition system to reservoir properties

§ Facies
§ Porosity and pore geometry
§ Permeability (absolute and relative)
§ Rock fluid interactions
§ Wettability and capillary pressures
§ Petrophysical rock types
36 © Alain Brie 2012 Advanced Formation Evaluation
36