04-Section 04 Pilot Testing & Contaminations
04-Section 04 Pilot Testing & Contaminations
section 4
introduction 2
designing pilot tests 2
pilot testing equipment 4
interpretation of pilot test results 4
rheological properties 5
retort analysis 6
filtrate analysis 7
cationic exchange capacity of clays 12
filtration 13
static aging 14
Section
Most chemical reactions require heat, mixing and time to drive the reaction. Therefore, it is necessary
to have a means for heating and agitating pilot test samples. Problems such as carbonates and
bicarbonates are not readily detectable and require a complete mud analysis and a pilot test series
with heat aging to determine proper treatment. Without heat aging, it is easy to over treat the
contaminant and create an even more severe problem. Ideally a portable roller oven should be
available at the rig site if extensive pilot testing is required.
Once the anomaly or anomalies of a drilling fluid’s characteristics have been identified via
conventional mud testing, the actual pilot test can begin. Guidelines that are fundamental to the
successful pilot test can be listed as follows:
1. On every test on which analysis is made, a control sample of mud should be taken.
2. If a combination of additives is to be tested, the effect of each additive on the mud should be
determined independently.
3. Some effects of additives will be observed almost instantly while other products may need a
minimum time (e.g., 4 hours hot rolling @ 150 °F or 65.6 °C) to determine their value.
4. Cost and availability of the products to be tested must always be considered in the final choice of
conditioning materials.
5. Duplicate the environment of each test as much as possible, i.e., use the same agitation (speed
and mixer), test temperature, volume, mechanical and electrical test devices, etc.
A pilot test sample should be representative of the fluid being used. Pilot testing is thus based on
the fact that 1g/350 cm3 of the sample is equivalent to 1 lb/bbl in 42 gal of the actual mud system.
ƒ temperature effects
ƒ drilling uncured cement
ƒ drilling anhydrite
ƒ encountering salt/saltwater flows
ƒ acid gas (CO2, H2S) intrusions
ƒ water on water-based mud contamination in oil-based mud
3. Adjustments to mud properties such as:
ƒ weight up/dilution
ƒ changing fluid loss properties
ƒ changing alkalinity/pH
ƒ treating carbonate/bicarbonate contamination
ƒ reducing hardness
ƒ adjusting MBT - clay content of the mud
ƒ changing oil/water ratio of oil muds
ƒ increasing electrical stability of oil muds
BARITE 42 gallons
100 lbs
(1.0 barrel)
100 lb
100 lb/bbl
42 gal
100.0 G
100 g
100 lb/bbl
350 cm3
To determine how to design a pilot test or test series, look at economics and potential for problems
down the road. For example, if you expect to encounter a pressured saltwater flow (16 lb/gal or
SG 1.92) with a 15 lb/gal (SG 1.80) freshwater mud at 350 °F (176.7 °C), the parameters for testing could
be:
Pilot test design requires calculating amounts of materials to put into the test samples. In pilot
tests, grams are equivalent to pounds and 350 cm3 is equivalent to one 42 gal oilfield barrel.
Material balance equations are used for pilot test design. For example, to weigh the 15 lb/gal
(SG 1.80) mud to 16 lb/gal (SG 1.92) without increasing the mud volume, one must calculate how
much 15 lb/gal (SG 1.80) mud to dump and how much barite to add to increase density. For simpler pilot
tests, such as adding only a few lb/bbl (kg/m3) treatments, it is not necessary to account for material
balance.
Section
Note: For liquid additives, volumes (gallons, cans, drums, bulk bags) must be converted into weights
(pounds, grams, millilitres) for pilot testing.
Rig site pilot tests have distinct practical advantages over sending a mud into the laboratory or
having a laboratory mud prepared for pilottesting. Rig site testing allows actual material and mud
to be used, which allows results to be readily available quicker (which is usually very important), and
allows the rig supervisor and the mud engineer to evaluate and review the pilot test results.
Laboratory pilot tests and planning are both important in preparing to drill a troublesome well.
Both should be done well in advance of anticipated problems. In this case, lab pilot tests are
advantageous in that they can be performed in advance, but then pilot tested again at the rig site
with the actual mud and chemicals.
Note: Protective eyewear (safety glasses or safety goggles) must be worn at all times when mixing
chemicals.
For every pilot test (single or series) a control sample must be run in parallel with the test
sample. A control sample is the base mud which has not been treated, but which is taken through
all the mixing, heating, rolling, etc. processes. The control is used to aid interpretation of results.
Data is compared between the control and test sample to sort out the effects due to treatment
versus mechanical effects (mixing, rolling or time of exposure).
For example, a mud engineer has an oil mud with a low electrical stability (ES). He pilot tests a
sample with 2 lb/bbl (2 g/350 cm3 ) additional emulsifier and shears it on the mixer for 10 minutes.
The ES is much higher than before. He also has run a control sample on the mixer for 10 minutes,
but without the additional emulsifier, and obtained almost the same higher ES. Was the emulsifier
responsible for the improved ES? No, in this case the shearing gave the improvement. Results of
pilot testing should be thoroughly reviewed before drawing conclusions. Often, one pilot test will
lead to another one or two tests before the answer is satisfactorily clear.
rheological properties
plastic viscosity
Plastic viscosity is proportional to rate of shear, thus largely reflects the resistance to flow due to
mechanical friction of the particles.
Plastic viscosity is a function of solids’ concentration and shape. It will be expected to increase with
decreasing particle size with the same volume of solids.
In oil muds, the plastic viscosity decreases with an increase in temperature or oil content.
ƒ Drilled solids
ƒ Rapid penetration rates with inadequate drilling solids control and extended drilling with a
PDC bit produce more drilled solids particles per unit of volume
ƒ Surface additions
ƒ Oil additions to water muds; water additions to oil muds; asphalt additions to water or oil
muds. Lost circulation materials; weighting materials, (e.g. graded calcium carbonate, barite,
ilmenite, iron carbonate, galena, etc.)
b) Cross reference
ƒ Dilution
ƒ Employment of mechanical solids removal devices
ƒ Surfactants (Water or oil wetting agents)
yield point
Yield Point is a function of the concentration of mud solids and their surface charges and potentials which
affect interparticle forces.
Dispersants and deflocculants are believed to adsorb on the mud particles. This action changes the
chemical nature of the surfaces and likewise affects the interparticle forces, resulting in viscosity and
YP reductions.
ƒ Flocculation due to soluble contaminants produced from formation (e.g., calcium, magnesium,
sulphides, carbon dioxide)
ƒ Surface Additives:
• Polymers
• Clays
• Surfactants
• Lubricants
• Lime
• Cement
• Detergents
• Lost circulation materials
ƒ Drilling hydratable shales
ƒ pH too low to solubilise deflocculants or dispersants
b) Cross References
ƒ Filtrate analysis
ƒ Methylene blue determination (CEC)
ƒ pH
Section
retort analysis
Determine percent by volume of oil, water and solids. Compare results with solids and average specific
gravity of solids graphs.
a) A frequent error encountered in the retort analysis is the result of loading the cell with gas-cut
mud. A higher solids content than actual is therefore calculated.
Causes for increases in the liquid phase originate from formation fluids or from surface additions
(inadvertent or on purpose).
Increases of solids can be caused by fast drilling rates, penetration of salts, sands or failure or
absence of solids separating devices.
b) Cross reference
ƒ
Rheometer - plastic viscosity
ƒ
Mud balance - rapid density fluctuation
ƒ Dilution.
ƒ Employment of mechanical solids removal devices (e.g., decanting centrifuges) and/or reduction
of screen size openings of shale shakers and mud cleaners.
Solids Check List for Diagnosing and Treating Non-Dispersed Mud Systems
Relative Proportion of Clay and Barite
filtrate analysis
Generally, the results from the filtrate analysis will confirm the departure from normal of the values
of yield point and gel strengths from rheological tests.
Increases in mud volume due to liquid or gas intrusions should also be noted. Salt water flows are
almost always accompanied by methane gas. Methane does not affect the chemical properties of
either oil or water-based muds. Hydrocarbon gases can thin an oil-based mud through becoming
dissolved in the base oil.
Sour gases (i.e. hydrogen sulphide and carbon dioxide), are generally found together, although rarely
in one to one proportions. When carbon dioxide is the major component of the intrusive gas, it will
mask the hydrogen sulphide. The reverse, however, is not true.
All salt water flows bring some calcium, magnesium, sodium and chloride ions into the mud.
High concentrations of magnesium chloride in water are not uncommon in North Sea drilling.
Water flows in other areas have shown high concentrations of calcium chloride.
In addition to gases and liquids, soluble formation salts can contribute to the contamination of the
mud system. The common ones encountered are :
ƒ Halite, rock salt, (NaCl)
ƒ Sylvite (KCl)
ƒ Tachhydrite (2MgCl2 - CaCl2 - 12H2O)
ƒ Anhydrite (CaSO4)
ƒ Gypsum (CaSO4 - 2H2O)
Calcite, CaCO3 (common name, limestone) and dolomite, (CaCO3 - MgCO3) are not considered
chemical contaminants because their solubilities are too low.
Cements are made from limestone and clay or shale. If the clay or shale does not contain enough
iron and aluminium oxides, these materials are added to the cement. The finely ground raw
material, either wet or dry processed, is fired in a rotary kiln and the carbon dioxide is driven
off. The resultant “clinker” is finely ground and mixed with small amounts of gypsum. This is the
basic “common cement”. Cement can be considered a contaminant, especially if it is entrained in a
water base mud before it has hardened or set. As much as 2% borax may be found in some
cements. Borax has an extreme viscosifying effect on some polymers, especially the guar family.
Section
alkalinity
Most contaminants with the exception of cement will lower the pH and/or alkalinity.
Virtually all water base muds perform better on the alkaline side of neutral. In addition, corrosion
is retarded by an alkaline environment. The exception is when aluminium drill pipe is being used in
which case the pH is controlled below 10 to prevent attack of the metal by hydroxyl ions.
Sodium carbonate (soda ash) and sodium bicarbonate precipitate soluble calcium in water-based
muds. Mud properties, after a continued use of either, become difficult to control. Poor filtration control,
high viscosity and gels and ineffectiveness of dispersants are a result of that treatment. The Pf-Mf
test is accurate for water but because muds contain ions other than hydroxyls, carbonates and
bicarbonate which interfere with the test, the back titration method (P, P1, P2) is preferred.
Pm (Pmud) is the test to determine the amount of alkalinity present from soluble caustic soda and
insoluble lime present in the mud.
Lime reacts with sodium bicarbonate to give caustic soda and a precipitate of limestone (CaCO3).
The product soda ash reacts with lime also to give limestone:
If the bicarbonate is present as calcium bicarbonate, lime treatment will remove it:
Lime will not always improve unstable muds high in bicarbonate probably due to the effect of
a high sodium concentration. There is no way to reduce this sodium concentration. Avoidance of
long periods of treatment with soda ash or sodium bicarbonate for soluble calcium is advisable.
Instead, the use of some lime is recommended. Similarly, maintenance of alkalinity with caustic soda
for prolonged periods should be avoided by switching to lime or using a combination of both.
ion analysis
a) Chloride - Cl-
In water muds, an increase in chlorides signifies the penetration of a salt water flow, formation
salt, or the swabbing of a salt water sand by sudden withdrawal of the drill pipe and bit in a near
gauge hole.
Dilution and restoration of the alkalinity are recommended. There is no chemical treatment to
precipitate the Chloride ion to render it ineffective.
b) Sulphate - SO4 - -
Sulphates are usually derived from formation waters and anhydrite or gypsum. “Gyppy” make-up
water is common in wells or stock tanks. Anhydrite and gypsum are found as formations in
many drilling areas. In the cap rock of salt domes, anhydrite and gypsum are commonly found.
Some drilling fluid products that contain sulphates are plaster of Paris (sulphate-hemihydrate),
gypsum, salt cake (sodium sulphate), and cement.
A result of excessive soluble sulphates in water-based muds is flash gels or high 10-minute
gels. An oilfield term, “soda ash gels”, is derived from the addition of soda ash to a water-based
mud, producing high gels when agitation ceases. The sodium ions react with soluble sulphates
to cause flash thickening of some polymers and clays.
Muds treated with chemical thinner and dispersant can tolerate high sulphates. Barium
carbonate can be used to convert the soluble sulphate to an insoluble precipitate of barium
sulphate if enough calcium is available to react with the excess carbonate of the reaction. EPM
of sulphate x 0.0346 equals the lb/bbl (x 0.0987 equals the kg/m3) of chemical treatment by
barium carbonate.
The Hach Meter is preferred to the test tube estimation for determining sulphate value even
though dilution of the filtrate sample is necessary.
Generally considered together, they are termed “total hardness”. Soluble calcium and magnesium
are found in salts and formation waters. They are common in make-up water whether it be
from the sea, producing wells, rivers, or stock ponds. The solubility of calcium is 600 - 800 ppm
when derived from gypsum and anhydrite.
Section
Most water based muds can tolerate 200 - 400 ppm of hardness. Filtration control is affected
by the calcium flocculating the clays and/or polymers in the drilling fluid. Magnesium reacts
generally the same with polymers. Exceptions exist however with certain high quality PAC
materials tolerating magnesium but not working very well with calcium in excess of 1,000
ppm. Calcium will affect the thinning performance of lignite also although it does not inhibit
the thinning ability of ferrochrome lignosulphonate.
Calcium can be precipitated from solution by several common chemicals. The choice depends
on conditions and the mud type (e.g. No hardness solubility would be anticipated in a high pH
lime mud.) They are :
Recommended for salty muds. Does not affect magnesium. Reacts with calcium to form
calcium sulphate (solubility of 600 - 800 ppm). Use only when calcium is in excess of 1000 ppm.
One lb/bbl will reduce calcium by about 800 ppm. Use of salt cake in fresh water muds is not
recommended for the reasons already described under “sulphate”. Salt muds are already
flocculated so increase of sulphates has little effect on mud properties.
Forms CaCO3 (limestone). About 0.2 lb/bbl (0.571 kg/m3) for every 200 ppm of calcium
Polyphosphates
Small amount of polyphosphates are used for light calcium contamination in fresh water muds.
The calcium is precipitated as an insoluble phosphate. Treatments should not in general exceed
0.5 lb/bbl (1.43 kg/m3).
Polyphosphates are unstable above 180 °F (82 °C) and can cause mud thickening.
10
d) Bicarbonates, Carbonates - HCO3- , CO3- -
Soluble carbonates or bicarbonates found in drilling fluids generally originate from these
sources ; (1) formation carbon dioxide gas, (2) make-up water, (3) decomposition of mud
products and (4) reaction products from the use of sulphide scavengers. Carbon dioxide in an
alkaline environment forms bicarbonate which then proceeds to the carbonate.
Carbon dioxide is generally found along with methane and hydrogen sulphide. Although
coexisting with hydrogen sulphide, it will sometimes mask it and go undetected in an alkaline
environment. Taking the carbonate from the above reaction, it is believed to react in the following
way:
Raising the pH is not recommended for treatment of soluble calcium derived from cement
contamination because pH is already high.
Reacts with soluble calcium to form limestone. Recommended for cement contamination
because pH is lowered and calcium precipitated.
Small amounts of carbon dioxide are derived from lignite subjected to high bottom hole
temperatures.
Soluble carbonates and bicarbonates can be converted to insoluble calcium carbonate through
the use of some form of calcium such as lime, gypsum, or calcium chloride. Generally, lime is used
although the pH will be raised. The gypsum or calcium chloride will affect pH very little but
will contribute sulphates and chlorides, respectively. Slight fluctuation may occur upon the entry
of any of the three if reactive clay content is high.
x 0.013 = lb/bbl
x 0.0371 kg/m3 Lime
x 0.024 = lb/bbl
x 0.0685 kg/m3 Gyp
x 0.025 = lb/bbl
x 0.0713 kg/m3 Calcium
Chloride (78%)
11
Section
Carbonates, which are reacting out, are generally evidenced after several minutes of stirring
through reduced viscosity and gels.
e) Sulphides - S--
f) Soluble sulphides are generally derived from the sour formation gas, hydrogen sulphide.
Packer fluids, but rarely drilling fluids, are attacked by sulphate-reducing bacteria which
produce sulphides. Some formation waters as well as crude oil contain sulphides that can possibly
contaminate muds. Some additives, such as liquid asphalt or other asphalt derivatives contain soluble
sulphides.
Flocculation of clay solids, increased viscosity, yield point, gels and filter loss, are some of the
effects of sulphide contamination. A decrease in alkalinity and a colour change (dark green to
black) of mud, along with a rotten vegetation or rotten egg odour are common symptoms of
a sulphide contaminated mud.
A useful general equation to determine the amount of H2S (ppm) a given mud can neutralise:
This is one of the most overlooked tests in the field but its significance related to viscosity,
filtration, filter cake quality, high temperature gelation, and drilling rate is very important. Sampling
and testing the cuttings using the same technique will produce an insight as to effect of the borehole
on the drilling fluid. The following table is a guide for clay content of four mud types.
lb/bbl kg/m3
Mud Wt 9 10 11 12 13 14 25.7 28.5 31.4 34.2 37.1 39.9
Non-dispersed low solids 14 14 14 13 12 10 39.9 39.9 39.9 37.1 34.2 28.5
Fresh Water Caustic lilgnosulphonate 26 24 22 20 18 16 74.2 68.5 62.8 57.1 51.4 45.6
GYP/ lignosulphonate 30 27 24 22 20 18 85.6 77.0 68.5 62.8 57.1 51.4
Lignite surfactant (204 ˚C) 16 15 14 13 12 11 45.6 42.8 39.9 37.1 34.2 31.4
lb/bbl kg/m3
Mud Wt 15 16 17 18 19 20 42.8 45.6 48.5 51.4 54.2 57.1
Non-dispersed low solids 9 8 8 - - 25.7 22.8 22.8 20.0 - -
Fresh Water Caustic lilgnosulphonate 14 12 10 8 7 6 39.9 34.2 28.5 22.8 20.0 17.1
GYP/ lignosulphonate 16 14 12 10 8 7 45.6 39.9 34.2 28.5 22.8 20.0
Lignite surfactant (204 ˚C) 10 8 6 4 3 2 28.5 22.8 17.1 11.4 8.6 5.7
12
The solution to the problem of excessive reactive clay entrained in the drilling mud can be approached
from two directions:
1. If more of the mud-making formation is to be drilled, a more inhibitive mud system would be
recommended.
filtration
The rate of loss through a cake is dependent upon particle size distribution in the mud and the
incorporation of droplets of water and/or oil in the openings between the solids. The openings
are controlled by the filtration control agents. The basic filtration control agent of many water base
muds is bentonite (whether it is to be as little as 3 - 4 lb/bbl (8.56 – 11.4 kg/m3) in low solids non-dispersed
muds, or as much as 25 - 35 lb/bbl (71.3 – 100 kg/m3) in seawater dispersed muds).
It should be noted that to have liquid loss, a porous medium must be present. The viscosity of the
filtrate has some effect also on rate of loss. Although shales are practically impermeable, hole stability
in some areas is directly related to liquid loss. Some shales are micro-fractured and the migration of
liquids through these passages has a lubricating effect. This effect is thought to occur in certain areas
using oil base mud. When the shales are steeply-bedded, semi-collapse of the borehole has been a result
of this phenomenon.
In some areas the chemical nature of the filtrate, rather than the amount, is more important as related
to shale stability. Importance is also attached to productivity of porous zones as affected by mud
filtrates.
1. The significance of increase in filtration at room temperature and 100 psi (690 kPa) pressure is that
it is associated with contaminants.
Increase in : Volume
Calcium
Magnesium
Sulphates
Chlorides
Increase in : Chlorides
Calcium
13
Section
ƒ Gypsum of anhydrite associated with massive beds or stringers and the cap rock of salt domes
Increase in : Sulphates
Calcium
ƒ Contaminants are often found in bulk products, such as barites and clays, due to carelessness in
transportation and handling.
ƒ Drilling personnel on offshore rigs have mistakenly pumped cement or seawater into the active
mud system.
ƒ Drilled solids, especially sand, can increase the filtrate. Some shales will reduce the filter loss.
2. Cross references to the increase in filter losses are almost always detected by increases in the viscosity
measurements and in the ion analysis of the filtrate.
3. The significance of increases in bottom hole temperature. 500 psi filtration losses are generally
associated with the lack of certain mud products or the thermal degradation of the products being
used. The presence of oxygen with some mud materials lowers their thermal stability. However, in
analysing a mud’s performance in regard to temperature, the following should be considered :
ƒ The amount of clay (bentonite) should be carefully observed. Too little can give high filter losses.
This can be the case where decanting centrifuges are being used on a regular basis. Excessive
clays however, can produce undesirable gelation and viscosity at elevated temperatures.
static aging
This test is an effort to duplicate the effect of temperature on the mud left in the hole during a trip
for a new bit, a logging run, running casing, or any other extended period of time when the pumps are
idle.
The standard cells are normally pressured to 500 psi (3449 kPa), or less, and that, in essence, is where
part of the test loses its credibility with oil muds. Tests have shown that pressure increases do not affect
the viscosity of water based muds. Oil based muds become thinner at higher temperature but more
viscous at higher pressures. Thus, the pressure partially offsets the effect of the higher temperature.
14
The significance of the test is that it indicates:
ƒ The degree of suspension to prevent weighting materials from settling under temperature
and pressure. This is very important for muds which are used as packer fluids. One of the criteria
for success is being able to pull the packer without having to wash down to the top of it.
ƒ The degree of trouble getting casing, logging tools, and drill bits to the bottom of the hole
after extended periods without bottom hole circulation. This indicator is the shear strength of the
aged sample.
ƒ Thermal stability after long-term aging with regard to filter loss. This is tested by both room
temperature, 100 psi psi (690 kPa) and HTHP filtrations.
ƒ The effect of temperature on the mud chemicals and resulting alkalinity.
ƒ The amount of fluid separating from the mud itself. This applies to oil muds only.
ƒ The effect of temperature on the degree of emulsification. This refers to oil muds only and
electrical stability specifically.
Suspension in several water based muds is generally related to the amount and type of commercial
clays used. Excessive drilled solids, bentonite, alkalinity, and temperature can form cement. Some
suspension as well as temperature stability regarding fluidity can be achieved with large amounts (15 - 30
lb/bbl or 43 – 86 kg/m3) of thinner (lignite) or leonardite (brown coal). Both are aids to filtration control
as well as suspension in hot holes. More modern fluids however rely solely on polymers for
suspension with bentonite added only in high temperature applications to provide desired filter cake
characteristics/fluid loss control.
Much success has recently been experienced in large diameter hole drilling, milling operations
and horizontal hole drilling using mixed metal hydroxide systems which demonstrate significantly
improved suspension characteristics and superior return permeability data.
Alkalinity must be maintained for good mud performance as far as corrosion, filtration, and fluidity
are concerned; but excess in alkalinity leads to high temperature gelation and / or solidification.
Decreasing the shear strength of a particular mud generally involves dilution, reduction of drilled
solids and/or commercial clays, adjustment of alkalinity, and increase in dispersant or deflocculant.
Top oil separation can be decreased by an increase of water content; additions of organophilic
clays (gellants) accompanied by some fluid loss additive; certain emulsifiers. This applies to oil muds
only.
Reduction of gellant content and drilled solids by oil dilution, accompanied by oil mud thinner and oil
wetter additions, will reduce excessive shear strengths of oil muds.
15