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CORE SAMPLE PREPARATION – AN INSIGHT IN TO

NEW PROCEDURES
M. Byrne and I. Patey, Corex UK Ltd

This paper was prepared for presentation at the International Symposium of the
Society of Core Analysts held in Abu Dhabi, UAE, 5-9 October, 2004

ABSTRACT
This paper aims to challenge many of the traditional methods employed in core analysis to
prepare core plug samples for testing. Studies over many years have revealed that different
lithologies can be altered in different ways during plug cutting, cleaning and drying.

Core plug samples for many core analysis measurements are removed from core and then
trimmed to create right cylinders. The cutting and trimming of core plug samples can
affect subsequent petrophysical measurements and some procedures will be proposed in
the paper derived from analysis of many different rock types.

For many core analysis measurements, samples are cleaned of pore fluids and
contaminants and then either measured in a dry state or with partial or full resaturation.
Cleaning and drying of rock samples can be achieved using many different techniques.
These techniques will be briefly reviewed and some new evidence presented which
demonstrates severe damage to different rock types caused by some commonly used
cleaning techniques. The development of a new modified Soxhlet cleaning technique will
be presented formally for the first time.

This paper will present laboratory data, supported by SEM analysis which clearly
illustrates the sensitivity of many different rock types to preparation techniques. Opinions,
strongly held and based on a weight of evidence will be presented and we expect the paper
to add to the already lively debate which exists on these topics.

INTRODUCTION
Core testing has many uses and applications in the oil industry. Reservoir capacity and
performance can be predicted and understood using core testing. Well performance,
development strategy and reservoir potential can also be examined. All core testing should
endeavour to measure real rock properties and minimise the impact of testing equipment
and core preparation procedures. Two factors which have been found to have significant
impact on some core measurements and which have not been satisfactorily addressed
previously are explored in this paper.

When core plugs are removed from core, they are usually cut as long cylinders and then
trimmed to right cylinders of appropriate length. Cutting the core and trimming creates
rock flour or “cuttings” some of which are usually deposited onto the core plug surface.
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This layer of debris can affect all measurements made on the core plug sample. Various
methods for removal of this rock flour have been proposed in the past. These include
brushing dry or under liquid, blowing clear with air or nitrogen and trimming whilst
flowing fluid out of the sample through the end faces. Other techniques which have been
used include “sellotape” peel or the use of a vacuum to remove rock flour. Brushing can
simply redistribute the flour and in some cases force it deeper in to the pores. Blowing
with gas can also force the rock flour deeper in to the pores. Trimming in a confining
device with flow can be laborious and can also promote fines migration. This paper
proposes a simple technique which effectively removes rock flour and does not have any
obvious disadvantages. This technique has been in regular use for more than ten years and
has been very successful in ensuring accurate subsequent core measurements.

The majority of reservoir rock samples available for testing are either poorly preserved or
not preserved. To proceed for testing they need to be cleaned of residual solids and fluids.
There are many different methods for cleaning samples and the selection of the optimum
method can have a profound effect on all results obtained from subsequent tests. One
popular method for cleaning is to flow fluids or combinations of fluids through the plug
samples in a core holder. Amongst the potential problems with this method are: potential
for fines migration to occur prior to the real laboratory testing; poor cleaning efficiency –
inefficient sweep of all pores; difficulty in achieving required saturation with subsequent
fluids. Hot Soxhlet solvent extraction can also be used to rapidly clean samples. This
technique is now largely discredited due to severe alteration to delicate minerals which can
occur. The photographs presented in figures 4 and 5 are adequate evidence to condemn
this technique where important decisions are to made on the basis of core testing. We
believe that the best cleaning/drying methods are cold static cleaning and warm constant
immersion cleaning. Cold static cleaning is normally prohibitively time consuming but
warm constant immersion achieves good results in reasonable time. Samples are dried by
low temperature oven drying to retain the intrinsic structures within the pore space.
Cornwall1 previously outlined how the continuous immersion technique can be used to
control the rate and aggression of the cleaning process. The method described in this paper
can be applied to all core samples in order to improve the quality of the cleaning process.

LABORATORY PROCEDURES
Acetate Peel To Remove Rock Flour
The method used for the removal of rock fines from the plug end faces is an adaptation of
the stained acetate peel technique described by Katz and Friedman2. Although this
technique was first used to produce rapid stained peels of limestones as a representative
thin section, by adapting the method to that described below, it has proved to be very
successful in removing the bulk of the rock flour from the plug end faces of sandstone and
carbonate rock types.

A square section of acetate sheet approximately twice the size of the plug end face
diameter is submerged completely in acetone solvent for up to 1 minute until it becomes
jelly-like. This is then attached to a dry acetate sheet square and as soon as the jelly
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acetate is attached to the dry acetate sheet, the wet surface is applied to the plug face and
rubbed gently until no air bubbles are observed. The plug plus acetate sheet is then left to
dry out at room conditions overnight. The acetate/acetone is allowed to harden or set. The
acetate sheet should then be carefully peeled off the end face of the plug, which should
now appear cleaner. A microscope can be used at this stage to ensure that the rock flour
has been removed successfully.
The acetate peel technique is used to remove rock flour from flat end faces and curved
surfaces of plugs and whole cores during cleaning. It can also be used to remove the
contaminating layer of debris from preserved or fully saturated samples although this
requires a small modification to the technique.

Figure 1. The upper Figure 2. The upper Figure 3. The upper

photograph shows the photograph shows the photograph shows the
plug face with no prior plug face after being plug face after being
treatment. Immediately brushed to remove loose acetate peeled, to remove
after the sawing and rock fines and appears rock fines from the pores.
removal of the plug end cleaner than the untreated When compared to
trims. Rock fines occur in face shown in Figure 1. Figures 1 and 2 the
patches over the face S.E.M. however, shows sample appears
producing a hazy effect. that all pores now contain essentially free of rock
The lower photograph rock fines (lower fines. The lower S.E.M.
shows that few pores photograph). The photograph confirms that
remain open (black brushing appears to have the pores are essentially
patches), most being forced rock fines into free of rock fines.
blocked by loose rock pores previously open in
fines. the untreated sample.
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The visual evidence presented in Figures 1-3 shows the removal of rock flour creates a
fresh uncontaminated rock surface. Petrophysical measurements in the laboratory have
confirmed that in some cases there is a direct impact on the absolute value of permeability
measured. The greatest concern is for advanced testing with liquids such as relative
permeability or formation damage testing. The data presented in table 1 shows that even
air permeability can be affected by end face cleaning. Three lithologies or rock types are
presented. In each case brushing the end face causes a small alteration in air permeability
but in the case of the fine grained low permeability sandstone and of the chalk sample,
permeability after acetate peel has significantly increased. This is due to the removal of
flow restricting rock flour on the samples end faces. A large database exists which
suggests that the litholigies most susceptible to end face rock flour damage are fine grained
sands / silts and carbonates (matrix permeability).

Table 1. Comparison Of Air Permeability. Uncleaned, Brushed And Acetate Peel End
Face Treatments.

Permeability to Air (mD)

Lithology Uncleaned Brushed Acetate Peel

Fine Grained Sandstone 7.18 7.16 7.56

Coarse Grained Sandstone 297 296 303

Chalk 1.83 1.84 1.92

Continuous Immersion Soxhlet Cleaning

The main objectives of this new design are to enable efficient solvent cleaning of core
samples without damaging delicate minerals such as fibrous clays. Evidence presented in
this paper and in many previous publications have shown that delicate minerals can be
damaged during drying3,4,5,6. Standard Soxhlet type cleaning involves many rapid drying
cycles and where speed of cleaning is the most important factor the potential damage is
unacceptable in most cases. Cold Static Solvent cleaning is probably the least damaging
method but normally the time involved is prohibitive. A compromise is required which
has all the non-damaging benefits of cold static cleaning and most of the efficiency of hot
Soxhlet cleaning. The method developed is called Continuous Immersion Soxhlet (CIS)
cleaning.

The CIS technique consists of a flask where solvent (any standard core cleaning solvents
have been used) is boiled. The vapour rises and is directed in to a condenser which sits
above the core sample chamber. Condensed solvent drips down in to the sample chamber
but is directed to the base of the chamber and percolates up from the base. The chamber is
heated and includes a stir bar which agitates the incoming solvent. Core samples are
placed on a perforated shelf which sits a few inches off the bottom of the chamber.
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An outlet at the top of the sample chamber, above the top of the highest core sample allows
solvent to run off back in to the original solvent boiling chamber. The set-up allows for
continuous circulation of solvent. In practice, fresh batches of clean solvent are introduced
periodically. Throughout the process the core samples are in contact with warm clean
liquid solvent thus enabling efficient cleaning with no damage to delicate minerals.
Following the continuous immersion cleaning, samples can be dried by critical point
drying or low temperature oven drying.

Figure 4 shows a sample cleaned using CIS Figure 5 shows a sample cleaned using
and dried at low (60ºC) temperature. traditional hot Soxhlet cleaning and dried in
Delicate illite clay fibres are maintained in a hot dry oven (120ºC). The illite clay
their original positions – no collapse has fibres have collapsed and in some cases
occurred. The sample and any subsequent appeared “singed” from the high
measurements are representative of the temperatures. This sample and any
reservoir. subsequent measurements are not
representative of the reservoir.

Table 2 shows a selection of results from extensive testing of various cleaning and drying
techniques. The data has been selected to demonstrate trends which have been observed
but also to show anomalies which exist in most core measurement data sets. The data
represents a comparison of standard hot Soxhlet cleaning and high temperature oven
drying with CIS and lower temperature drying. All of the samples illustrated contain
fibrous illite clay with percentages of bulk rock from 0.8% to 4.3% (determined by XRD
with qualification by SEM). In general, the data shows that hot Soxhlet cleaning of fibrous
illite clay rich samples leads to an increase in measured permeability. There is a
reasonable correlation between the amount of this clay type and the observed increase in
permeability. The main exception to this rules is sample 5 where the illite clay was later
observed to have remained standing proud across all pores and no evidence of collapse was
seen. Figures 4 and 5 are taken from sample 3 and clearly show collapse of illite clay as
the reason for the increase in permeability. No changes in grain density were observed for
these samples and small increases in porosity were sometimes observed.
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Apparent porosity increases may be due to removal of tiny pores in between clay fibres
due to collapse or might indicate migration of collapsed clay fragments.

Table 2. Comparison of Base Parameters - Samples cleaned and dried in conventional

soxhlet / hot air drying and sample cleaned by C.I.S. and dried at 60°C.

Fibrous Illite as Permeability to Air

Sample % Bulk Rock Porosity % Grain Density g/cc (mD)
(XRD) Conv C.I.S. Conv C.I.S. Conv C.I.S.
1 2.1 22 22 2.64 2.64 317 294
2 0.8 25.6 25.5 2.65 2.65 380 382
3 2.9 18.4 18.1 2.65 2.65 60.3 48.4
4 4.3 21.2 21 2.67 2.67 13.9 10.2
5 1.8 16.5 16.4 2.65 2.65 19.4 19.4

CONCLUSIONS
Many techniques used in standard core preparation can affect the subsequent
measurements made on those cores. This paper outlines two significant improvements in
sample preparation which have been successfully developed and implemented. A selection
of data and photographs presented in this paper have indicated that the use of these new
techniques can have a major impact on petrophysical measurements. With continued
vigilance and development we can help to improve understanding of reservoir properties
and performance and produce laboratory data which accurately represents real reservoirs.

REFERENCES
1. Cornwall, C.: 2001. The Preservation or Removal of Solid Bituminous Material,
as part of the Core Analysis Programme on the Elgin-Franklin Field: SCA 2001-
48
2. Katz, A and Friedman, G.M.: The preparation of stained acetate peels for the
study of carbonate rocks: 1965.
3. Pallatt, N. Wilson, J. and McHardy, B.: The Relationship between Permeability
and the Morphology of Diagenetic Illite in Reservoir Rocks: 1984 SPE 12798.
4. Gant, P. and Anderson, W.: Core Cleaning for Restoration of Native Wettability:
1988 SPE 14875
5. Morrow, N. Cather, M., Buckley, J and Dandge, V.: Effects of Drying on Absolute
and Relative Permeabilities of Low-Permeability Gas Sands: SPE 21880 1991
6. Mikkelsen, M. Scheie, A., Rong, Q and De Boer, E.T.: Abnormal Permeability
Behavior of a North Sea Sandstone Reservoir: 1991 SPE 22600.