03-Section 3A WBM Testing

testing
section 3
mud testing procedures

section 3a - wbm testing procedures section
section 3b - naf testing procedures

Section
3
mud testing procedures
health, safety and environment
Mud Engineers will be responsible for ensuring that all mud testing activities are carried out in a safe
and responsible manner, especially those involving high pressures, high temperatures and dangerous
chemicals. Be aware of the hazards and ensure that all risks are well managed.
Mud Engineers will be responsible for ensuring that all hazardous testing chemicals are correctly
labelled, and safely stored and handled. They will also ensure that testing chemicals sent off the rig are
correctly packaged and labelled.
MSDS sheets for all the mud testing chemicals should be available in the mud lab. Copies should also be
distributed to the Medic, client representative and the contractor representative.
Empty bottles of testing chemicals should be thoroughly flushed out with water and then returned to
the Mud Company for re-cycling or disposal.
A Hazchem poster should be posted in the lab, detailing all the mud testing chemicals:
ƒ Product Name
ƒ Colour Code
ƒ UN Code
ƒ First Aid Treatment
ƒ Fire Fighting Media
ƒ Action for Spillage
ƒ Personal Protection Recommended
It is recommended to have a pair of oven gloves available for handling hot testing equipment, eg. retort
and HTHP.
Safety glasses are mandatory when conducting any mud test. This will help protect the eyes from
broken glass, or being splashed with chemicals, mud or mud filtrate.
Pipette filling devices are recommended for titrating, as they will prevent any dangerous chemicals
being swallowed.
Mud engineers should ensure that the mud lab has an adequate method of extracting fumes from
chemicals or retorts. Either a strong extractor or a fume cupboard is recommended. If fume extraction is not
adequate then recommendations for its improvement should be submitted to the client representative.
If the mud lab is sited in a designated hazardous area the mud engineers should ensure that the mud
lab is suitably pressurised. If pressurisation is inadequate then recommendations for its improvement
should be submitted to the client representative.
An adequate number of power points of the correct voltage should be available in the mud lab.
Power points that have too many appliances running off them are a common source of fire. If there are
not enough power points often a request to the rig electrician can resolve the matter. If that is not
successful then the client representative should be consulted.
Any base oil, or synthetic or ester based mud samples that are used for testing should be kept and
disposed of in the active mud system. It should not be flushed down the sink.
If practical, the surfactant mixtures that have already been used for testing non water base muds should
be kept in a suitable container and later sent to shore for appropriate disposal.
Surgical gloves should be available for handling dangerous testing chemicals or non water base fluids.
Section
3 mud testing procedures
good laboratory practices

Regularly calibrate mud balances, pH, electrical stability and K+ meters.
Ensure that all testing equipment is kept clean, working properly and that spare parts are available.
This is particularly important in reference to “O” rings, batteries, gaskets, pressure regulators, HTHP
valves, and meter probes.
For critical instruments like the 6 speed Viscometer, it is necessary to have a back up 6 speed Viscometer,
or handcrank available.
All bottles of titrating chemicals must have a manufactured date on them. The date will indicate
whether the chemical is still fresh enough to return accurate results. Ensure that a good supply of
fresh testing chemicals is available. If there is any uncertainty about the accuracy and/or age of a
particular chemical compare results obtained using a fresh sample of the same chemical. Ensure, where
applicable, that all testing chemicals, including Dräger tubes and stick chemical testers, eg. nitrates and
sulphites are within their use by date.
Always use a dedicated, labelled pipette for each testing chemical. This prevents cross contamination
of testing chemicals and erroneous test results.
After use the WBM filtrate sample pipette should be flushed with distilled water and allowed to dry
before re-use. This prevents salt crystals forming on the tip of the pipette.
Use 50 ml glass beakers stirred with a small magnetic bead on a hot plate/stirrer in preference to the
traditional ceramic or plastic titration dish and a glass rod stirrer. This method is far simpler and will
lead to more consistent results.
Wash all glassware with distilled water after use and drain dry or dry off with a clean paper towel.
Keep the mud lab clean and tidy.

section 3a
wbm testing procedures

section 3a Scomi Oiltools
mud density 2
funnel viscosity 3
rheology 4
retort analysis 7
api filtrate 10
hthp filtration 11
sand content 13
pH 14
filtrate alkalinity – Pf and Mf 16
filtrate hardness – Ca++ and Mg++ 18
filtrate chlorides 20
phpa content 22
potassium ion – direct reading potassium ion meter 25
potassium ion – sodium perchlorate method
(steiger method) 26
mbt test 27
glycol – cloud point and % by vol concentration 29
garrett gas train - sulphides 30
garrett gas train - carbonates 34
silicate testing 37
Section
3a wbm testing procedures
wbm testing procedures

mud density
discussion
The Mud Balance is used for mud weight determinations and is the
recommended equipment in the API 13B standard procedures for testing
drilling fluids. The mud balance is accurate to within +/- 0,1 lb/gal (or 0.5
lb/cu.ft, 0.01 g/ml, 10 g/l). It is designed such that the mud cup, at one end
of the beam, is balanced by a fixed counterweight at the other end, with a
sliding weight rider free to move along the graduated scale. A level bubble is
mounted on the beam to allow accurate balancing.
This, most basic, of mud properties is often reported incorrectly due to the
use of an inaccurately calibrated mud balance. The time to check the balance
is not when a well control situation develops but on a routine daily basis.
The mud test kit will contain both standard mud balances and a pressurised
Halliburton mud balance. Both types are calibrated by weighing distilled
Have you
water at 70 °F (21.1 °C) and obtaining a reading of 1.00 SG / 8.345 lb/gal. If checked the
this is not the case adjust the balance by adding or removing lead shot as mud balance
required. lately?
Experience has shown that, under normal drilling conditions, the standard
balance gives the same reading as the pressurised balance. For ease of use,
therefore, the standard balance may be routinely used to measure mud
density.
At the first indication of gas or air entrapment in the mud only the pressurised
balance should be used.
On a per tour basis the pressurised balance will be used to confirm it is reading
the same as the standard balance
equipment
ƒ Standard Mud Balance
ƒ Pressurised Mud Balance
procedure – standard balance

1) Instrument base must be set on a flat level surface.
2) Measure and record the mud temperature.
3) Fill the mud cup with the mud to be tested. Gently tap the cup to encourage
any entrapped gas to break out.
4) Replace cap and rotate until it is firmly seated, ensuring some of the mud
is expelled through the hole on top, to free any trapped gas.
5) Holding cap firmly (with cap hole covered
with thumb) wipe the outside of the cup
until it is clean and dry.
6) Place the beam on the base support and
balance it by using the rider along the
graduated scale. Balance is achieved
when the bubble is directly under the
centre line.
Example of standard mud balance

procedure – pressurised balance
A problem with many drilling fluids is that they contain considerable amounts
of entrained gas, leading to inaccurate mud weight measurements on the
standard mud balance. By pressurising the mud cup the entrained air volume
can be decreased to a minimum. The balance operates in much the same way
as standard mud balance except the lid of the mud cup has a check valve.
1) Follow steps 1 - 5 as for the standard mud balance procedure.

2) Place the lid on the cup, with the valve in the open position, wipe the
outside of the cup clean and dry.
3) The pressurising plunger is similar to operating a syringe. The plunger is
filled by submersing the nose of the plunger in the drilling fluid with the
piston rod in the completely inward position. The piston rod is then drawn
up, thereby filling the plunger with fluid.
4) The nose of the plunger is then placed into the female ‘O’ ring on top of
the cap. The sample is pressurised by maintaining a downward force on
the cylinder housing in order to hold the check valve open, whilst at the
same time forcing the piston rod inwards. Approximately 50 pounds of
force or greater should be maintained on the piston rod.
5) The check valve in the lid is pressure actuated, i.e. closing as pressure is
applied. The valve is therefore closed by gradually easing up on the cylinder
housing while maintaining pressure on the piston rod.
6) Having applied pressure to the sample with the pump there should be no
indication of fluid leaking back through the nipple. It should not be possible
to depress the nipple by hand – if the nipple can be easily depressed it
is a sign that pressure is not being held and a true weight is not being
obtained. Change the ‘O’ ring and repeat the test.
7) Once the check valve is closed, disconnect the plunger and weigh the fluid
as in step 6 of the standard mud balance procedure.
interpretation
The density of WBM does not vary greatly with temperature. However, it is still
a requirement to report the density at flowline and ambient temperatures.
Water based muds can be prone to air entrapment and foaming. It is important
to ensure that the density reported is as accurate as possible. The reason for
this is that under downhole conditions the mud is compressed and thus the
effective mud weight at the bottom can be much higher than indicated by a
gas cut surface sample.
Do not weigh up mud to compensate for an aerated or gas cut surface sample
– Ensure you have a true mud weight before doing anything.
For density control purposes the mud weight will always relate to what is
being measured at flowline temperatures as this is the best indicator of what is
actually in the hole at any particular time.
funnel viscosity
discussion
The Marsh Funnel Viscometer is used for routine viscosity measurements. The
results obtained are greatly influenced by rate of gelation and density. The
latter varies the hydrostatic head of the column of mud in the funnel. Because
of these variations, the viscosities obtained cannot be correlated directly with
those obtained using the rotational viscometers, and therefore can ONLY be
used as an indicator of mud stability, or relative changes to mud properties.

Section
The funnel viscosity will be measured in seconds per quart.
The funnel must be calibrated on a regular basis. The viscosity of fresh water
at 70 °F (21.1 °C) is 26 secs/qt (27.6 sec/l) and any reading above this would
indicate that the spout of the funnel required cleaning. The diameter of the
spout is 3/16” and a hand held drill bit of this diameter should be used to clear
any deposits/cake.
equipment
ƒ Thermometer: 32 – 220 °F (0 – 105 °C)
ƒ Stopwatch
ƒ Graduated cup: one quart / litre
ƒ Marsh funnel
procedures
1) Cover the orifice with a finger and pour a freshly agitated fluid sample
through the screen into the clean, dry and upright funnel until the liquid
level reaches the bottom of the screen.
2) Quickly remove the finger and measure the time required for the fluid to
fill the receiving vessel to the one quart (946 ml).
3) Report the result to the nearest second as Marsh Funnel viscosity and the
temperature to the nearest degree.
interpretation
The funnel viscosity is a good quick guide to whether a water based mud
is thickening or thinning. However further analysis of rheology and solids
content will be required before embarking on any treatment program.
The result is temperature dependent but not to the same degree as SBM.
The funnel viscosity is, therefore, a more relevant indicator of trends in a

WBM.
rheology
discussion
The rheology will be determined using a Motor Driven Fann 6 speed
Viscometer. Ensure that the Viscometer motor runs at the same electrical
cycles (either 50 hertz or 60 hertz) as the rig power, otherwise erroneous
readings will be obtained. Offshore rigs usually operate on 60 hertz.
All Viscometers sent to the rig site must have been recently calibrated and When checking oil
carry a label noting the date of the last calibration. base mud systems it is
recommended to insert
the thermometer in the
Drilling fluid is contained in the annular space between two concentric actual fluid to ensure
cylinders. The outer cylinder or rotor sleeve is driven at a constant rotational the correct testing
velocity. The rotation of the rotor sleeve in the fluid produces a torque on temperature has been
the inner cylinder or bob, and the dial attached to the bob indicates reached
displacement of the bob. This is the standard procedure recommended by
API 13B for field testing water based drilling fluids.
Instrument constants have been adjusted so that the Bingham plastic

viscosity and yield point can be obtained by using the readings at 300 rpm
and 600 rpm.

The six readings will be taken at 120 °F (48.9 °C). A heated cup will be
used for this purpose. Water Based Muds exhibit thinning tendencies with
temperature and so it is still necessary to standardise this test by taking the
readings at the same temperature on each occasion.
The thermometer used must be calibrated against a mercury or alcohol

type thermometer to confirm its accuracy. To adjust the thermometer
simply use a small spanner to turn the nut on the back of the dial so that
the thermometer reads the same temperature as the mercury or alcohol
thermometer.
The rheometer readings may be taken at a higher temperature, to reflect flow

line temperatures, if required. However, to avoid confusion and to allow
comparisons between wells, usually only the 120 °F (48.9 °C) readings will be
entered in the mud check columns on the mud report. If necessary, readings
taken at higher temperatures can be noted in the comment section.
Note: Maximum operating temperature is

200 ˚F (93 ˚C). If fluids above 200 ˚F
(93 ˚C) are to be tested, a solid metal
bob or a hollow metal bob, with
completely dry interior, should be
used. Liquid trapped inside a hollow
bob may vaporise when immersed in
high temperature fluid and cause the
bob to explode.
The gelling characteristics of the fluid can

be determined from taking a 10 second
and a 10 minute gel reading. Consequently
there is no requirement to take a 30 minute
gel under normal circumstances. However Example of 6 Speed
if increasing rheology is becoming a Rheometer
problem a 30 min gel should also be taken
in order to determine the effectiveness of
the treatment programme.
equipment
ƒ Fann 35, 110 volt or 120 volt, powered by a two speed synchronous motor
to obtain speeds of 3, 6, 100, 200, 300 and 600.
ƒ Mud cup
ƒ Stopwatch
ƒ Thermometer 32 – 220 °F (0 – 104 °C)
procedures
1) Stir the sample at 600 rpm while the sample is heating, or cooling, to 120 °F
(48.9 °C). Ensure the dial reading has stabilized at this speed before noting
the result and proceeding to the 300, 200, 100, 6 and 3 RPM speeds.
2) Having taken the 3-RPM reading stir the sample at 600 RPM for 30 secs
before taking the 10-second gel at 3 rpm.
3) Restir the sample at 600 rpm for 30 seconds and leave undisturbed for
10 minutes, ensuring the temperature stays at 120 °F (48.9 °C). Take the
10 minute gel reading at 3 rpm.

Section
calculations
Apparent Viscosity (AV) in = 600 reading ÷ 2
Centipoise (cps)
Yield Stress = 2 x 3 reading – 6 reading
Plastic Viscosity (PV) in = 600 reading - 300 reading

Centipoise (cps)
Yield Point (YP)

Yield Point (YP) in Ib/100 ft2 = 300 reading – PV
Yield Point (YP) in Pa = (300 reading – PV) x 0.48

Power Law Index (n) = 3.32 log (600 reading / 300 reading)
Consistency Index (K):

n
Consistency Index (K) in Ib/100 ft2 = 600 reading / 1022
n
Consistency Index (K) in Pa = (600 reading / 1022 ) x 0.48
Gels:
Gels in Ib/100 ft2 = As per 10 sec & 10 min reading
Gels in Pa = (As per 10 sec & 10 min reading) x 0.48
Note: If the 600 rpm reading is off scale then the PV and YP can be calculated
as follows;
YP in Ib/100 ft2 = (2 X 100 rpm reading) – 200 rpm reading

YP in Pa = [(2 X 100 rpm reading) – 200 rpm reading] x 0.48
PV = 300 rpm – YP
300 rpm reading – YP
PV (S.I units) =
0.48
interpretation
The main focus of attention, with regards to mud rheology, is the 6 rpm reading.
Mud programs will specify a range for the 6 rpm reading and so the other
indicators of rheological properties, i.e. yield point, apparent viscosity, plastic
viscosity and initial gel strengths, become a function of what is required to meet
this low end specification.
Experience has shown that the initial gel strength will be more or less the same
as the 6-rpm reading.
10 minute gels that show an increasing trend and a widening divergence from
the initial gel are a good indicator of a colloidal solids build up that may not be
detected by solids analysis. This is due to the fact that while the solids percent
may remain the same the actual size of the particles, and hence the surface area
they present to the liquid phase, will decrease as degradation occurs.
If the colloidal solids increase is not due to reactive claystones then the MBT
test may not reveal the true nature of what is happening. The 10 minute gel
in a WBM will always react to increasing fines and can often be the best indicator
of solids related changes to mud properties.
Increasing PV values are also generally a good indicator of a solids build up.

It is important to identify increasing trends at an early stage so that timely
measures may be taken before they reach problem levels.
retort analysis
discussion
The accurate determination of the high gravity solids and low gravity solids
in a WBM mud relies on the correct usage of the 50 ml retort and the correct
interpretation of the results.
A retort is used to determine the quantity of liquids and solids in a drilling fluid.
A carefully measured sample of mud is placed in a steel cell and then heated
until it vaporises. The vapours are then passed through a condenser and
collected in a calibrated cylinder. The volume of liquid, water and oil can then be
calculated in percent. The percent solids value, both suspended and dissolved,
is determined by subtraction of the total liquid from 100%.
Small errors in the measurement of the solids percentage can result in seriously
erroneous reporting of the drilled solids content. It is apparent that inaccurate
retort results can lead to unnecessary mud treatments aimed at reducing an
apparently out of spec LGS concentration.
It is essential that the retort be run at a high enough temperature to burn off
the heavier fractions of any liquid additives such as glycol or lubricants.
It is absolutely critical that the correct mud weight is used in the calculation
to determine the relative concentrations of HGS and LGS. Using the flowline
mud weight when the sample to be retorted has in fact cooled considerably,
and hence increased in density, will give a much higher LGS content than
is actually the case. The retort mud weight, i.e. the actual density of the mud
in the retort as opposed to the flow line mud weight, will, therefore, be utilised
in all calculations.
The volume of the retort will be confirmed by filling the cell with distilled
water (at ambient temperature) and checking that 50 cc’s is in fact received in
the test tube. If 50 cc’s is not consistently obtained with distilled water (it might
be necessary to repeat the check with distilled water to ensure the error is
genuine) then, either the 50 cc retort cell must be replaced with an accurate
one, or, a correction factor must be applied to the volume of distillate actually
obtained, as per the following formula:
50
x Volume of distillate ccs
Volume of distilled water obtained ccs
Any smoke emerging from the heating jacket is an indication that vapour is
escaping through the threads connecting the upper and lower parts of the
retort cell. If this is noted it is an indication that the tube to the condenser is, or
has been, blocked. A blocked tube will result in the bottom of the upper part
of the retort cell “flaring” to allow an escape route for increasing pressure. Even
if the tube is subsequently cleaned the flaring will remain and is still an
escape route for a proportion of the vapour. This will obviously result in an
inaccurate solids measurement. Any hint of smoke from the heating jacket
is an indication that the top part of the retort cell is damaged and should be
discarded.

Section
It can be appreciated that a combination of all, or some of the factors

mentioned above, i.e. insufficient retort temperature, incorrect mud weight
used in calculations, volume being retorted not in fact 50 cc’s, partial escape
of vapour through flared threaded area, can result in wildly inaccurate
determinations of the drilled solids content.
equipment
Three retort sizes are available to the industry, 10 ml, 20 ml and 50 ml. The
latter is recommended for drilling operations, due to its greater precision and
accuracy. Each unit consists of;
ƒ Sample cup
ƒ Thermostatically controlled heating element
ƒ Liquid condenser
ƒ Pyrex measuring cylinder (50 ml)
ƒ Fine steel wool
ƒ Pipe cleaner
ƒ High temperature silicone grease
ƒ Defoaming agent
ƒ Spatula
procedures
1) Ensure retort assembly to be used is clean
and dry. It is vital that all traces of previously
retorted solids are removed from the retort
cup to guarantee 50 ml of fluid is actually
retorted. Remove all traces of previously
used steel wool. Water can be retained in
steel wool when the upper retort body
is washed / cleaned. Failure to change
the steel wool can result in inaccurate Example of Retort
measurements, as this extraneous water
will become included in the total water content.
2) Weigh the clean and dry retort cup and lid on the triple beam balance.
3) Add the mud, which has been allowed to cool to ambient temperature,
to the retort cup, gently tap the cup to remove any air bubbles and place
the lid with a rotational movement to obtain a proper fit. Be sure an excess
of fluid flows out of the hole in the lid.
4) Carefully clean the cup and lid of excess fluid and reweigh on the triple
beam balance. The retort mud weight SG is determined as the difference
between the empty and full weights, in grams, divided by 50 (the volume of
mud).
5) Pack the retort body with new steel wool, apply Never–Seez, to the threads
and assemble top and bottom parts. Ensure that the two parts are fully
screwed together. If it is not possible to fully screw together the two parts it
will be necessary to clean the threads and repeat the above steps. Failure to
get a good seal could result in leakage that will lead to an inaccurate result.
6) Attach the condenser and place the retort assembly in the heating jacket
and close the insulating lid.
7) Place clean, dry liquid receiver below condenser outlet and turn on heating
jacket.
8) The temperature control should be adjusted so that the retort cell glows
dull red at the end of the distillation. Ultimately smoke will emerge from
the retort and the distillation is only complete when the smoke stops.

calculations
SG of drilled solids (LGS) = 2.60
SG of Barite (HGS) = 4.25
SG of oil additive = SGo
Input Data
SG of mud in retort = SGm

Retort % oil = Of
Retort % water = Wf
Retort % solids = Sf
mls of 0.282NAgNO3 x 10,000
Salinity mg/l =
% Water ÷100
SG of Brine = SGb (Look up Salinity in
specific brine table)
Correction factor = CF (From brine table)
Brine fraction = Bf (Correction factor x Wf)
Corrected Solids = CS [Sf - Salt content (Bf - Wf)]
Then…
SGm x 100 - [(Of x SGo) + (Bf x SGb)]
Average SG of Solids =
CS
(AVSG)
CS x (4.25 - AVSG)
% LGS =
4.25 - 2.6

= CS x (4.25 - AVSG)
1.65

% HGS = CS - % LGS
lb/bbl LGS = %LGS x 3.5 x 2.6
= %LGS x 9.1
lb/bbl LGS = %HGS x 3.5 x 4.25
= %HGS x 14.87
kg/m3 LGS = %LGS x (9.1 x 6.2897) ÷ 2.205
= %LGS x 25.96
kg/m3 HGS = %HGS x (14.87 x 6.2897) ÷ 2.205
= %HGS x 42.42
interpretation
The control of the low gravity solids content of a WBM system will trigger
the use of centrifuges or dilutions. If mud costs were broken down and assigned
to a particular reason then the control of LGS would probably account for the
bulk of expenditure on most wells. For this reason very careful attention must
be paid to the points outlined in the Discussion section above.
This test is a reliable indication of the condition of a drilling fluid on a one

off basis. The results of other tests may change, for example, with shear and
temperature i.e. the rheology may increase, the API filter loss may decrease
without any additions being made to the mud. The LGS content, however, is
something that can be assessed, and tackled if required, without waiting for
trends to be established from further tests.
The calculations are extremely sensitive and a 0.5% difference in total solids
content will have a large affect on the LGS fraction. For this reason it is
important to be meticulous when taking the volumes of oil, water and solids.

Section
api filtrate
discussion
Filtration control is one of the primary characteristics of a drilling fluid and
fulfils a variety of functions from the prevention of differential sticking to
minimisation of formation damage.
Filtrate control can be established at just about any level but the cost increases
almost exponentially as tighter and tighter properties are required. A fit for
purpose attitude must be adopted when programming fluid loss levels to
avoid non-justifiable expense. No benefit may be gained, for example, from
having a fluid loss of 3 ml as opposed to 5 ml but mud costs will have doubled.
Further, over treatment with fluid loss polymers, especially PAC polymers,
can have a detrimental effect on the rheology by reducing the mud’s shear
thinning characteristics.
The API test for WBM is carried out at ambient temperature and with only
100 psi (690 kPa) of differential pressure. This quite patently does not mirror
downhole conditions. However experience has shown that this test is a reliable
way of measuring the performance of a drilling fluid at any given moment.
The results must be viewed in conjunction with the thickness of the filter
cake that has been formed by the end of the test. A low solids polymer mud
may have a relatively high fluid loss but the filter cake is almost non existent
whereas a high solids mud may have a lower fluid loss but a much thicker
filter cake.
equipment
ƒ Filtration Cell
ƒ OFI specially Hardened Filter paper - Filtration Area 7.07 sq.in (Alternatively
- Whatman No 50 paper)
ƒ Low Pressure CO2 supply 100 psi (690 kPa) (Soda stream cartridges)
ƒ Stop Clock
ƒ 10 and 25 ml measuring cylinders
procedure
1) Assemble the clean and dry components that form the cell of this piece of
equipment.
2) Ensure the filter paper is Whatman no 50 (or equivalent) and make sure
the screen is not damaged. A creased screen can result in weaknesses in
the filter cake that seem to result in higher results than would normally be
expected.
3) Pour the mud sample into the cell to 0.5” from the top, put the top in place
and position it in the support frame.
4) Place a dry graduated cylinder of suitable size (usually 10 cc’s) under the
drain tube and apply 100 psi of pressure over 15 seconds.
5) Maintain a constant 100 psi (690 kPa) throughout the test period.
6) After 7.5 mins measure and record the amount of filtrate collected to the
nearest 0.1 ml.
7) After 30 mins measure and report the amount of filtrate collected to the
nearest 0.1 ml.
8) Having bled off the pressure, dismantle the equipment and examine the
filter cake. Report the thickness in 32nds of an inch (mm). Comments about
the quality of the cake should be noted in the comments section of the
mud report i.e. texture, colour, hardness, compressibility, flexibility etc.
10
calculations
API Fluid Loss = 30 min Reading
* Relative API Fluid Loss = (30 min Reading - 7.5 min reading) x 2
Spurt Loss = API Fluid Loss - Relative API Fluid Loss
* Relative API Fluid Loss is corrected for spurt loss prior to cake formation.
interpretation
The API fluid loss may not give an accurate representation of what is
happening under dynamic conditions at downhole temperatures and
pressures. Dynamic lab testing has shown solids content to be the key
influencing factor. Thus it could follow that a mud that has lower API fluid
loss than another may have a much higher dynamic loss.
However any change in fluid loss properties is a good indicator of general

mud health. Having established the required control any increasing trend must
be identified and treated as required.
Fluid loss can also decrease without any chemical additives as solids content
and particle size distribution optimises under drilling conditions.
Generally speaking, therefore, an increasing trend is bad and a decreasing trend

is good.
The results must be viewed in conjunction with the thickness of the filter cake
that has been formed by the end of the test. A low solids polymer mud may have
a relatively high fluid loss but the filter cake is almost non existent whereas a
high solids mud may have a lower fluid loss but a much thicker filter cake.
hthp filtration
discussion
The high pressure / high temperature filter press is a static filtration procedure
recommended by the API 13B standard procedures for testing drilling fluids
at elevated temperatures and pressures.
This test tends to be run at temperatures that reflect expected bottom hole
temperatures and thus there is no standardised temperature. However ensure
the test temperature is noted on the mud report.
These procedures are for temperatures up to 300 °F (148.9 °C). If higher test
temperatures are required a porous stainless steel disc will need to be utilized
instead of the normally used filter paper and higher top and bottom pressures
applied. When heating, apply 100 psi (690 kPa) to top and bottom, increase top
pressure to 600 psi (4138 kPa) for the test.
The thermometer used must be calibrated against a mercury or alcohol type

thermometer to confirm its accuracy. To adjust the thermometer, simply use a
small spanner to turn the nut on the back of the dial so that the thermometer
reads the same temperature as the mercury or alcohol thermometer.
Remember the screen and bomb are a matched pair. The use of unmatched
pieces of equipment may result in it being impossible to get a result as whole
mud breaches the seals at some point during the test. This is indicated when
the pressure gauge on the bottom pressure vessel suddenly goes off scale.
11
Section
Remember the screen and bomb are a matched pair. The use of unmatched
pieces of equipment may result in it being impossible to get a result as whole
mud breaches the seals at some point during the test. This is indicated when
the pressure gauge on the bottom pressure vessel suddenly goes off scale.
Continuing bypass problems could be the result of incorrect ‘O’ rings. Ensure
they are of a rounded, rather than flat, profile
equipment
ƒ HTHP Filtration Cell
ƒ OFI specially Hardened Filter paper
ƒ High Pressure CO2 supply 600 psi (4138 kPa)
ƒ Stop Clock
ƒ 10 and 25 ml measuring cylinders
procedure
1) Turn on heated jacket at the mains and insert
a thermometer into the jacket and leave to
preheat to the desired temperature.
2) Check out all the “O” rings on the HPHT bomb
and lid. Change out any damaged rings. The
rings to be checked are the four small stem “O”
rings, which tend to pick up cuts and grooves
with time, and the two large “O” rings, one in
the lid and one in the cell. The large “O” rings
should have a rounded profile and be free from Example of HTHP
Filter Press
dirt.
3) With stem valve closed on bottom of cell, fill up cell with mud to within
0.5” of the ‘O’ ring groove, to allow for thermal expansion.
4) Insert filter paper into the cell followed by the bottom cell plate assembly
over the filter paper and twist to align with the safety locking lugs. Ensure
the lid stem is open while doing this to avoid damaging the filter paper. Do not use nitrous oxide
5) Tighten the 6 grub screws evenly using the Allan key provided. (N2O) as a pressure
6) Ensure all stem valves are tightly closed. source for this test. N2O
7) Invert cell and place in filtration mounted heated jacket assembly. can detonate when
under temperature
Rotate the bomb until it seats on the locking pin. Insert a thermometer
and pressure in the
into the HPHT cell. presence of oil, grease, or
8) Place a CO2 or N2 cartridge in each regulator and tighten up the retainers. carbonaceous materials.
9) Place the pressure unit on top valve and lock into place using a locking Use only carbon dioxide
pin. Lock the bottom pressure unit to the bottom valve into place, again (CO2) or nitrogen (N2).
ensuring that locking pin is inserted.
10) Apply 100 psi to both ends of the HPHT cell with the valves still closed.
11) Open the top valve by turning 1/4 to 1/2 anticlockwise to apply 100 psi to
the mud while heating to prevent the mud from boiling prior to reaching
the target temperature. The time for heating the mud sample to the
target temperature should not exceed 60 minutes!
12) When the cell reaches the required test temperature open the bottom
stem (1/2 turn) and then increase the pressure on the top regulator to If the bottom pressure
600 psi over +/- 20 seconds. rises 20 psi above the
13) Commence the test. The test should be carried out as soon as the bomb specified pressure during
reaches the test temperature. the test, carefully bleed
off pressure by draining a
14) If the pressure on the bottom regulator increases significantly above 100
small volume of filtrate.
psi bleed off some of the filtrate into the graduated cylinder.
12
15) Collect the filtrate for 30 minutes maintaining the temperature to within
+/- 5 °F (2.7 °C).
16) Once the test has finished close the top and bottom valves and shut off the
pressure supply from the regulators. Bleed the lines using the relief valves
provided.
17) Allow filtrate to cool for 30 minutes and then draw off into a graduated
20 ml measuring cylinder and read volume. SAVE the filtrate for ionic
analysis.
18) CAUTION - the cell still contains 500 psi (3449 kPa) pressure, so cool cell
to room temperature ideally in a water bath or alternative safe place and
then bleed off the pressure slowly by opening the valves.
19) Disassemble the cell and discard mud into mud waste container only. Save
filter paper handling with care and wash filter cake with a gentle stream
of distilled water.
20) Measure and report the thickness of the cake to the nearest 1/32” (0.8 mm).
Report any other observations, such as texture, colour, hardness, flexibility
etc.
calculations
The total filtrate volume should be doubled, as the standard API press is
twice the area of the HPHT cell.
Mud in the filtrate would indicate that the ‘O’ ring seals needed replacing as
whole mud was bypassing the filter paper.
Do not instigate mud treatments on the results of any test that has mud in
the filtrate. Overhaul the equipment and repeat the test.
sand content
discussion
It is important to remember that this test is a measure of sand size particles,
which can be of any rock type, or indeed sacked additives, as opposed to just
sand.
If finer than 200 mesh shaker screens are in use, an increase in sand size
particles would be a clear indicator of screen damage requiring immediate
attention.
equipment
ƒ 2 1/2” inch diameter sieve (200 mesh, 74 micron),
ƒ Plastic funnel to fit the sieve
ƒ Glass measuring tube marked for the volume of mud to be added in order
to read the percentage of sand directly in the bottom of the tube, which is
graduated from 0 to 20%.
procedures
1) Fill the tube with mud to the mark
labelled “Mud to Here”, and then add
water to the mark “Base Fluid to Here”.
Cover the mouth of the tube with the
thumb and shake the tube vigorously.
Example of Sand Content Kit
13
Section
2) Pour the suspension through the clean, dry mesh screen, being careful
to remove all solids out of the tube by flushing with base fluid back
through the same mesh screen. By tapping the side of the screen the
pouring of the mud through the screen may be facilitated.
3) Wash the sand retained on the screen with water to remove any remaining
mud
4) Fit the funnel upside down over the top of the sieve, invert slowly turning
the tip of the funnel into the mouth of the tube and wash the sand back
into the tube with some clean water. Allow the sand to settle.
5) Record the quantity of sand settled in the graduated tube as the sand
“sized” content of the mud in percent by volume.
calculations
Allow the sand to settle. From the graduations on the tube, read and report
the percent by volume of sand size drilled solids (see interpretation below).
interpretation
Some interpretation of the result will need to be made based on the
differential settling speeds of the different materials present. The reported
result should be that proportion of the settled particles that are attributable to
drilled solids. These would be the particles that settle out first and are usually
followed by calcium carbonates, other types of LCM and undissolved black
powders. The differing particles aggregate, therefore, in clearly identifiable
strata and, depending what was being added to the active system at any given
time, the apparent sand content can appear much higher than it actually is.
The sand content is not really of any significance with respect to overall mud
properties but is of importance when it comes to wear on mud pump parts
etc. 2% is normally accepted as the upper limit.
Generally speaking the sand content is also useful to gauge the effectiveness
of the shaker screen sizes being employed. If the sand content rises quickly
then this is an indication that finer mesh screens need to be tried. A rapid
increase in sand content over a short period can also indicate that the shaker
screens are torn and need immediate replacing.
pH
discussion
Field measurement of drilling fluid (or filtrate) pH and adjustments to the pH
are fundamental to controlling water-based drilling fluid properties.
pH expresses acidity or alkalinity of an aqueous solution. An acid can be

defined as a substance which dissociates in aqueous solution to give hydrogen
[H+] ions, whilst a base or alkali gives [OH-] ions. The term “pH” denotes the
negative logarithm of the hydrogen ion, [H+], activity in aqueous solutions
(activity and concentration are equal only in dilute solutions).
The pH of a water based mud is controlled to improve the performance of

mud additives, to minimise pipe corrosion and to reduce the solubility of
claystones.
A balance is struck between these factors when choosing a pH for any

particular system.
14
Generally speaking for low pH muds eg KCl / PHPA, 8.5 to 9.5 are the norm.
At these levels:
ƒ Sufficient alkalinity is maintained to control corrosion, i.e. the mud is not
acidic.
ƒ Polymer additives are not co-precipitated with other ions and hardness is
minimised.
ƒ The dispersive tendencies of claystones are minimised, thus helping to
prevent solids problems.
It is important to remember that pH is a logarithmic function and that it will
take 10 times as much caustic soda (in pure water) to increase a pH from 10 to
11 as it will from 9 to 10.
The recommended method for pH measurement is with a glass electrode

pH meter. This method is accurate and reliable, being free of interferences if
a high quality electrode system is used with a properly designed instrument.
Rugged pH instruments are available that automatically temperature
compensate the slope and are preferred over the manually adjusted
instruments.
For anything other than basic freshwater mud systems a pH meter should
be used to measure pH.
Note: Colour matching pH paper and strips are used for field measurements,
but are not recommended as they are only reliable in very simple water
base muds. Mud solids, dissolved salts and chemicals, and dark coloured
liquids cause serious errors in pH paper values. Readability is normally
about 0.5 pH units.
equipment
ƒ pH Meter: Millivolt range potentiometer calibrated to show pH units for
measuring the potential between a glass membrane electrode and a
standard “reference” electrode.
ƒ Electrode system: A combination system of a glass electrode for sensing
[H+] ions and a standard voltage reference electrode (silver/silver chloride),
constructed as a single electrode.
ƒ Buffer solutions: Three solutions to calibrate and set the slope of the pH
meter prior to sample measurement.
ƒ pH = 4.0: potassium hydrogen phthalate at 0.05 molar in water. Gives 4.01
pH at 75 °F (23.9 °C). Only use fresh
ƒ pH = 7.0: Potassium dihydrogen phosphate at 0.02066 molar and disodium calibration fluids
when calibrating
hydrogen phosphate at 0.02934 molar in water, gives 7.00 pH at 75 °F (23.9 °C).
the pH meter
ƒ pH = 10.0: Sodium carbonate at 0.025 molar and sodium bicarbonate at
0.025 molar in water, gives 10.01 pH at 75 °F (23.9 °C).
Note: The shelf life of all buffers should not exceed six months before disposal.
Date of preparation of the buffer should be shown on bottles used in the
field. Bottles should be kept tightly stoppered.
ƒ Distilled or deionised water: in spray bottle.

ƒ Soft tissues: to blot electrodes.
ƒ Thermometer: glass, 32-220 °F (0-105 °C).
15
Section
procedures – pH indicator strips

1) Place an indicator strip in mud and allow it to remain for one minute to
allow the colour to stabilise.
2) Rinse the strip off with deionised water but do not wipe.
3) Compare the colours of the strip with the standard chart provided and
estimate the pH to the nearest .5.
procedures – pH meter
1) The pH meter must be calibrated, as per the manufacturer’s instructions,
on a regular basis (at least once a week, more frequently if meter usage is
high. Buffer solutions used must be within their use by date. Do not
re-cycle the buffer solutions used to calibrate the meter. Throw them away
each time and use fresh samples of the buffer solutions every time the
meter is calibrated.
2) For accurate pH measurements the test fluid, buffer solutions and
reference electrode must all be at the same temperature i.e. ambient
temperature.
3) Insert the electrode into the fluid contained in a small glass flask and swirl
gently.
4) Measure the fluid pH according to the directions supplied with the
instrument. When the meter reading becomes constant record the pH to
the nearest 0.1 of a unit.
5) Thoroughly clean off electrode with distilled water and store it in
accordance with manufacturer’s recommendations.
interpretation
Trickle treatments of either sodium hydroxide or potassium hydroxide are
usually made to maintain the pH in the optimum range of 8.5 to 9.5. A quick
check with the pH meter will avoid a situation where pH increases above this
range due to over treatment or drops too low due to under treatment.
The usual tendency is for the pH to drop slowly as alkaline ions are neutralised
by other naturally occurring ions. A rapid drop in pH can indicate such hazards
as acid gas or CO2 influxes.
filtrate alkalinity – Pf and Mf

discussion
Alkalinity can be considered as the acid-neutralising power of a substance.
Alkalinity measurements can be made on either the whole mud (designated
with the subscript m) or on the filtrate (subscript f ). The data collected
can also be used to estimate the concentrations of hydroxyl (OH-), carbonate
(CO3--) and bicarbonate (HCO3-) ions in the drilling fluid.
Pf and Mf refer to titrations performed on the mud filtrate (f ). The P refers to

the indicator Phenolphthalein and thus Pf refers to the mls of 0.02N sulphuric
acid required for the indicator colour change at a pH of 8.3.
The M refers to the indicator Methyl Orange and the Mf is the mls of 0.02N
sulphuric acid for the colour change that at occurs at a pH of 4.3.
The Mf includes the acid taken to get to the Phenolphthalein end point and so
will always be equal to, or greater than, the Pf.
16
In colourless filtrates the Pf is a distinctive end point from red pink to
colourless. The Mf however is a very poor endpoint, orange to pink, much
dependent on the eye of the beholder, and casts into doubt alkalinity
calculations based upon it.
Another indicator, Bromo Cresol Green, changes from blue to apple green and
is a much easier end point to see. For historical reasons it is still referred to as
the Mf. It is this indicator, Bromo Cresol Green that will be used to calculate Mf.
The following table highlights the “rules of thumb” for conventional gel based
mud systems.
Hydroxyl ions Mud stable and in good condition

Hydroxyl + Carbonate Stable and in good condition
Carbonate Unstable but can be controlled
Carbonate + bicarbonate Stable but difficult to control
Bicarbonate Unstable and very difficult to control
Knowledge of the mud and filtrate alkalinity is essential to ensure proper

control of mud chemistry. Mud additives, particularly some deflocculants,
require an alkaline environment to function properly. The source and nature
of the alkalinity is often as important as the fact that some alkalinity exists.
Alkalinity arising from hydroxyl ions is generally accepted as being beneficial,
while alkalinity resulting from carbonates and/or bicarbonates may have
adverse effects on mud performance and stability.
equipment
ƒ Sulphuric acid solution: standardised 0.02 Normal (N/50).
ƒ Phenolphthalein indicator solution: 1 g dissolved in 60 ml ethyl or methyl
alcohol made up to 100 ml with distilled water.
ƒ Methyl Orange Indicator solution: 0.2 g dissolved in 100 ml distilled
water.
ƒ Bromo-phenol Blue (Bromo-cresol Green): 0.02 g in 100 ml distilled water
(instead of methyl orange for dark filtrates).
ƒ pH meter: optional, but is more accurate than indicator solution.
ƒ Titration vessel: 100 - 150 ml. preferably white.
ƒ Volumetric pipettes: 1 ml.
ƒ Graduated pipettes: one 1 cc. and one 10 ml
ƒ Hypodermic syringe: 2.5 ml.
ƒ Distilled water free of carbon dioxide (by boiling)
ƒ Stirring rod.
procedures
1) Measure one ml of filtrate into a clean and dry 50 ml glass beaker.
2) Dilute with 10 - 20 mls of distilled water.
3) Add 2 or three drops of Phenolphthalein indicator. If the sample turns
pink, add 0.02N sulphuric acid drop by drop from a pipette while gently
stirring with a small magnetic bead on a hot plate/stirrer until the pink
colour just disappears.
4) If the sample is so coloured that the colour change of the indicator is
masked, the endpoint is taken when the pH reaches 8.3, as measured with
the glass electrode pH meter.
5) Report the Phenolphthalein alkalinity as the mls of acid required to reach
the end point.
17
Section
6) To the same sample add 3 or 4 drops of Bromo Cresol Green. A blue colour
will develop.
7) Add 0.02N sulphuric acid drop by drop from a pipette while gently
swirling or mixing until the blue colour changes to apple green.
8) The Mf is the total amount of acid used for both titrations.
interpretation
Historically great effort went into interpreting the relationship between
Pf and Mf as a means of detecting some of the factors causing mud instability
such as high gels or deteriorating fluid loss properties.
Carbonates and Bicarbonates are usually responsible when analysis shows

an increasing Mf. They can be incorporated due to:
ƒ Over treatment with soda ash or bicarb to remove calcium or cement
contamination.
ƒ Carbon Dioxide dissolution due to formation gas, fluid mixing equipment
etc
ƒ Thermal degradation of organic materials such as polymers
ƒ Contaminated Bentonite and Barite.
It is true that carbonate and bicarbonate ions can have severe effects on
conventional kinds of water base mud systems, particularly gel based ones.
The inherent inaccuracy in the second end point determination makes

accurate analysis very difficult.
Other alkaline materials can also contribute to the overall alkalinity, further
complicating interpretation. These include but are not exclusive to anions
such as, borate, silicate, aluminate, sulphide and phosphate.
If Carbonate or Bicarbonate contamination is suspected it must be confirmed

and quantified by use of a Garret Gas Train.
In most applications Pf should always be greater than zero, i.e. always have
some pink colour, and the closer the Mf is to the Pf the better.
Experience shows, however, that in low solids polymer muds an increasing

Mf does not necessarily result in any affect at all on other key mud properties
such as filtration and viscosity.
The focus should, therefore, be on observing changes in fluid loss and

rheology and if unwanted changes are occurring see if they are related to an
increasing trend in Mf and treat accordingly.
filtrate hardness – Ca++ and Mg++

discussion
The ions that contribute most significantly to hardness in water are Calcium
and Magnesium. These ions are divalent and can act as bridging agents
between ionic polymers by complexing with more than one charged group
on the molecule. This bridging can reduce polymer solubility and hence
adversely affect performance.
18
In a similar manner the divalent ions can bridge between two clay particles
producing flocculation.
When EDTA (sodium salt of ethylene-diaminetetracetic acid) is added to

aqueous solutions containing calcium and/or magnesium, it combines to
form a complex whose end-point is determined by a suitable indicator.
EDTA-Na + Ca++ + Mg++ ----> EDTA- Ca + EDTA- Mg + Na+
Keeping the mud alkaline with trickle treatments of hydroxides will ensure
no magnesium is present. The OH– ion will react with free magnesium to
give an insoluble precipitate of magnesium hydroxide. Thus in a properly
maintained system, where an excess of OH– ions exist, no free magnesium
can exist and all hardness is due to calcium.
If huge sources of Magnesium are encountered then it is pointless trying

to keep adding hydroxides, as the increasing amounts of fine precipitates will
eventually result in uncontrollable viscosity increases.
In situations where hydroxide additions have no effect on pH and free

magnesium is present the system must be run at neutral pH, as the lesser
of evils.
equipment
ƒ 0.02 N EDTA (0.01 M) (Versenate Solution)
ƒ Ammonia Buffer* in dropper bottle
ƒ 8N Potassium hydroxide buffer (KOH)
ƒ Manver Indicator (solution or crystals)
ƒ Calver II Indicator (crystals)
ƒ Masking agent** : 1:1:2 mixture by volume of triethanolamine :
tetraethylenepentamine : water
ƒ Deionised water : free of carbon dioxide by boiling
ƒ Graduated pipettes: one 1 ml, 2 ml and 5 ml
ƒ Titration vessel : 100 - 150 ml preferably white
ƒ Stirring rods
* Ammonia buffer = 54 g Ammonium chloride and 400 ml Ammonium
hydroxide (15 N) made up to 1000 ml with deionised water.
** 1 ml of Masking agent should be added if soluble iron is suspected to

be present.
procedures – total hardness

1) This test measures the total hardness, calcium, magnesium and other
metals (of no real significance for drilling fluids) precipitated by Versenate
solution, of the mud filtrate.
2) To a clean and dry 50 ml glass beaker add 50 ml of distilled water and 2 ml
of standard buffer solution.
3) Add 1 ml of Calmalgite / Manver indicator solution.
4) If a red colour develops, indicating the presence of calcium or magnesium,
add Versenate solution (0.01M EDTA – 1 ml = 400 mg/l.) drop wise with
a pipette until the colour first changes to a brilliant blue, while stirring
with a small magnetic bead on a hot plate/stirrer.
This would indicate your distilled water was contaminated or the
titration vessel was not clean. Do not include this amount of versenate in
calculations.
19
Section
5) Measure 1 ml of mud filtrate into the titration vessel and the red colour
will reappear.
6) Add Versenate solution as before until the blue colour returns. The end
point may appear as a purple brown if masking agents are present.
However it is the clear colour change that is the end point.
calculations – total hardness

Total Hardness in mg/l (expressed as calcium) = ml of versenate solution x
400
procedures – calcium
1) To a clean and dry 50 ml glass beaker add 1 ml of filtrate (the purity of
the distilled water and your ability to clean a titration vessel will have been
proved in the previous procedure) and add 50 ml of distilled water and 5
ml 8N KOH or NaOH.
2) The OH¯ ions will precipitate out any magnesium.
3) Add a satchel (or a pinch if loose powder is provided) of Calver II calcium
indicator. This will produce a pink to a wine red coloration.
4) While stirring with a small magnetic bead on a hot plate/stirrer add
standard Versenate solution (0.01M EDTA – 1 ml = 400 mg/l.) until the
solution changes to clear blue.
calculations – calcium
Calcium hardness in mg / lt. = ml of versenate x 400
calculations – magnesium
Magnesium hardness in mg / lt. = (ml of versenate for total hardness test - ml
of versenate for calcium test) x 0.243
Interpretation
Keeping hardness levels under control improves the efficiency of water based
mud systems.
Remember, in a properly maintained alkaline system where excess OH– ions

exist, free magnesium cannot exist and all hardness will be due to calcium.
The acceptable upper limit for hardness is pH dependent but in systems run at
pH 8.5 to 9.5 the upper limit should be no more than 600 mg/l.
Remember that elevated hardness levels may not impinge at all on mud
properties such as filtration and viscosity but due to lowered efficiency levels
you are spending more money to achieve the same results.
Control calcium hardness with suitable treatments.
filtrate chlorides
discussion
This standard method (Mohr’s method) consists of titrating all chlorides
present in the filtrate and expressing the result in terms of sodium chloride.
This explains why in some cases, for example in the presence of calcium
and magnesium chlorides, the result obtained (expressed in NaCl), can
20
give concentrations greater than the solubility of NaCl. The chlorides are
precipitated in the form of silver chloride, in the presence of an indicator,
potassium chromate. The reaction occurs in two steps:
Cl- + AgNO3 → AgCl (white precipitate) + NO3-

CrO4-- + 2Ag+ → Ag2CrO4 (orange-red precipitate)
The end point is detected with Potassium Chromate.
The excess Ag+ ions present after all the Cl- ions have been removed from
solution, react with chromate to form silver chromate, an orange-red
precipitate. Since AgCl is less soluble than Ag2CrO4 the latter cannot form
permanently in the mixture until the precipitation of AgCl has reduced the
Cl- to a very small value.
Note: This titration must be carried out in a neutral medium because; in an acid
medium the silver chromate dissolves, and in an alkaline medium silver
oxide or silver carbonate precipitate. In practice, as the filtrate is neutral
or alkaline, it is first acidified with sulphuric or nitric acid, then neutralised
with calcium carbonate. The addition of the nitric acid has the advantage
of discolouring the filtrate (partially).
Numerous papers have been generated explaining different ways of reporting

salinity mg/l Cl-, ppm KCl etc. This has caused great confusion in the past
where apparently wildly different figures were in fact conveying exactly the
same salinity.
It is essential that salinity be always reported as mg/l chlorides. Remember

ppm is not the same as mg/l, (ppm x brine SG = mg/l)
equipment
ƒ Silver nitrate solution: 4.7910 g/l (0.0282 N or equivalent to 0.001 g chloride
ion/ml). Store in amber or opaque bottle.
ƒ Potassium Chromate Indicator solution: 5 g/100 ml water.
ƒ Sulphuric or nitric acid: standardised 0.02 N (N/50).
ƒ Phenolphthalein indicator solution: 1 g/100 ml of 60% alcohol in water
solution.
ƒ Calcium Carbonate: precipitated, chemically pure grade.
ƒ Distilled water: free of carbon dioxide by boiling.
ƒ Graduated pipettes: one 1 ml and One 10-ml.
ƒ Titration vessel: 100 - 150 ml preferably white.
ƒ Stirring rod.
procedures
1) Ensure the filtrate sample pipette doesn’t have any crystallised salt on its
tip. Measure one ml of filtrate into a clean and dry 50 ml glass beaker.
2) Dilute with 25 mls of distilled water.
3) Add three drops of Phenolphthalein indicator. If the sample turns pink,
add 0.02N sulphuric acid drop by drop from a pipette while gently
stirring with a small magnetic bead on a hot/plate stirrer until the pink
colour just disappears.
21
Section
4) Add 10 drops of standard potassium chromate solution (5 gms in 100 mls

of distilled water). A yellow colour develops.
5) Stir continuously while adding 0.0282 N or 0.282 N silver nitrate (depending
on expected range – below 5000 mg/l use 0.0282 N and above use 0.282
N) on a drop by drop basis.
6) The end point is reached when a reddish tinge appears and persists for
30 seconds. Do not titrate to “brick red” as this is too far past the end
point.
7) Note the amount of silver nitrate required to reach the end point.
calculations
Report the chloride ion concentration of the filtrate in mg/l, calculated as
follows:
1000 x (0.0282 N silver nitrate, ml)

Chloride, (mg/l) =
filtrate sample ml
Or when using 0.282 N silver nitrate
10000 x (0.282 N silver nitrate, ml)

Chloride, (mg/l) =
filtrate sample ml
To convert units:
(Chloride, mg/l) ___

Chloride, (ppm) =
Specific gravity of filtrate
Salt (NaCl), mg/l = (1.65) x (Chloride, mg/l)
interpretation
The Cl– ion does not deplete, so once a system has been established the
concentration should remain constant.
Any variation in established concentration could be indicative of a; fresh

or salt-water flow, seawater or freshwater additions, planned or evaporite
formations being drilled.
Chloride level on its own is not a reliable indicator of the amount of active ion
(potassium) present and so more emphasis should be placed on the specific
test for that ion.
phpa content
discussion
PHPA (partially hydrolysed polyacrylamide) is a polymer specifically designed
to provide encapsulation of claystone cuttings, thus preventing dispersion
and facilitate solids removal on surface.
Very high molecular weight, long chain anionic polymers are selected and the
adsorption of these chains at numerous positively charged sites around the
clay cutting results in a gelatinous coating which retards the movement of
water into the clay and consequently slows the processes of hydration.
22
Further to this a viscous filtrate is produced which slows water penetration
into the formation.
The requirement for PHPA is dependent on the types of formations to be

drilled and the ROP experienced. PHPA will be depleted constantly and once
a new system has been circulated into the well and initial screening problems
have passed the concentration should rapidly be increased to program
requirements.
As drilling continues it will be necessary to constantly add PHPA to maintain

levels and hence optimise the inhibitive environment.
Regular monitoring is required to ensure sufficient free polymer is available

in the fluid achieve the expected results. The test involves connecting two
Erlenmeyer flasks with a rubber tube. One flask contains the sample to be
tested and the other a mixture of boric acid and methyl red indicator. At the
end of the test the acid / indicator mix is titrated to determine the amount of
PHPA that was in the sample.
ƒ Hot plate magnetic stirrer

ƒ 2 x 125 ml Erlenmeyer flasks
ƒ Magnetic stirring bar
ƒ Distilled water
ƒ 2% by weight Boric acid solution
ƒ Methyl red indicator
ƒ 6 N Sodium Hydroxide solution
ƒ 2 - 3 ft (0.6 - 0.9m) of Tygon tubing
ƒ #6 rubber stopper with a 1/4” hole
ƒ 0.02 N sulphuric acid solution
ƒ Silicon defoamer (i.e. Dow-Corning 84, AFC-78)
ƒ 2 x 1/4” OD glass tubing each 3 or 4 inches (7.5 - 10 cm) long
procedure
1) Attach the two glass tubes to the ends of the Tygon tubing and fit one
of them into the rubber stopper so the end of the tube just fits flush with
the bottom of the stopper.
2) It is important the glass tubing be flush with the bottom of the rubber
stopper. If the glass tube protrudes below the stopper the caustic solution
being distilled will collect around the exposed tube and be sucked up and
over to the boric acid solution. This will lead to erroneous results.
3) To one flask add 25 ml of the Boric acid solution and 6 drops of methyl red
indicator. The solution will turn a red / pink colour. If an ammonia
4) To the other flask add 50 mls of distilled water, 2 ml of silicone defoamer odor is detected
and 5 mls of whole mud. as the solution
5) If foaming is a problem, or the mud bumps over, more defoamer can be in the flask boils,
immediately
used for the next test.
stop the test. An
6) Place the flask containing the mud on the hot plate/stirrer and begin ammonia odor
stirring. indicates leakage
7) Add 3 mls of 6N sodium hydroxide solution and immediately fit the flask from the flask
with the rubber stopper.
8) Submerse the other end of the tubing into the boric acid/methyl red
solution and begin heating the mud sample.
9) Ensure the receiving flask is at a lower level than the one being heated to
allow the distillate to run downhill.
23
Section
10) Heat for 60 minutes during which time approximately 20 to 25 ml of

distillate should collect.
11) The temperature setting at which to distil should be so as not to cause
boil over (which invalidates the test), but to give a gentle boil which
causes distillate to condense at the top of the glass tubing. Hence the
distillate isn’t boiled across but merely collects in the tubing and runs
down to the boric acid solution. Do not try to adjust the temperature
too much during heating as it can induce a pressure differential and
suck back the distillate, invalidating the test. Experience will show what
temperature setting on the hot plate is the most effective. Once this has
been established simply set the hot plate to that setting and leave it for
the duration of the test.
12) The boric acid solution should now be yellow.
13) Titrate the acid back to its original starting colour with the 0.02 N sulphuric
acid solution and record the amount of acid used.
calculation
The result will be read from a standard graph that has been prepared using
a known concentration of the particular PHPA to be used. It is recommended
to use powdered PHPA, as this is usually 100% active, whereas liquid PHPA
usually has between 30 – 40% active constituent.
Example of PHPA concentration curve
Example of PHPA Concentration Curve

2.5
2.0
PHPA (lb/bbl)
1.5
1.0
0.5
0.0
1 2 3 4 5 6 7 8 9 10
Millilitres of N50 Sulphuric Acid
interpretation
This test will establish the rate at which PHPA is being depleted from the
system and thus allow the treatment rate to be varied accordingly.
Maintaining the correct level of PHPA will decrease overall mud expenditure
by reducing the amount of dump and dilute treatments required to maintain
key mud properties such as filtration and viscosity.
As well as regularly doing this test it is essential to observe the cuttings at the
shakers. The cuttings should have a glossy appearance and remain discrete
when squeezed into a ball and then released. If this is not the case then,
no matter what the test result indicates, the PHPA concentration should be
increased.
24
potassium ion – direct reading potassium ion
meter
discussion
Potassium chloride is added to water based muds as source of potassium
ions. The potassium ions have a dehydrating effect on potentially swelling
clays by exchanging with sodium ions on the active clay surfaces.
While drilling reactive formations potassium ion levels can deplete while
chloride levels remain constant. It is apparent therefore that the mud must be
checked specifically for excess potassium.
The actual level of potassium required to provide adequate fluid inhibition

is dependent on the level of exchangeable ions in the formation clay and to
a lesser extent on the make up water. A higher level is required in seawater
based fluid in order to overcome the competitive effect of the sodium present
in the seawater. For this reason it is better for KCl / polymer type muds to be
freshwater based.
An Orion PerpHecT Model 370 meter or similar is suitable for use offshore.
This method is intended to be used for the analysis of filtrate samples only and
NOT whole mud samples!!
procedure
1) Carefully assemble and condition the electrode as per manufacture’s
instructions.
2) Calibrate the meter using known Potassium standards (ref manufacture’s
instructions). These standards should span the expected Potassium
concentration range to be measured. They should be prepared by diluting
0.1M Potassium Standard solution with distilled water. Use accurate
glassware and pipettes for all measurements. Ensure they are all thoroughly
clean and dry before use. It is recommended to check the meter’s calibration
every couple of days and to make fresh calibration standards every well.
3) Take 1 ml of mud filtrate sample and dilute with distilled water to reduce
the concentration to within the range of the calibration standards. Add
manufacturers recommended amount of Potassium ISA to sample as this
will ensure correct pH and reduce the effect of interfering ions. Ensure all
glassware is thoroughly cleaned with distilled water and dried before use.
It is important to realise that it is very easy to contaminate a test sample by
dirty glassware.
4) Stir all standards and samples at a uniform rate during measurement. It is
not recommended to use a magnetic stirrer as it may generate sufficient
heat to change solution temperature.
5) Samples or standards should be measured at ambient room temperature
for best results.
6) Always rinse electrode thoroughly with distilled water after use and store as
per manufacturer’s instructions. Do not wipe or rub the electrode’s sensing
membrane as you may contaminate and damage the surface.
calculations
Direct reading Potassium ion meters return direct Potassium concentrations.
Simply multiply the result by the dilution factor used on the filtrate sample to
obtain the actual filtrate Potassium ion concentration. Formulae or charts can
be used to convert the results into KCl % by wt, ppb or mg/l. etc.
25
Section
interpretation
The test reveals the rate of potassium exchange by reactive clay surfaces.
Again the test must be viewed in conjunction with the observed condition of
the cuttings at the shakers. Soft and unconsolidated cuttings could indicate an
increase in potassium level was required even though the test may indicate the
programmed concentration was present.
potassium ion – sodium perchlorate method

(steiger method)
discussion
As potassium ion – direct reading above
The test is not as accurate as the specific ion meter but has proved useful for
revealing trends and should be used where a meter is unavailable or out of
service.
The test involves precipitating potassium, centrifuging the precipitate formed

and then comparing the volume with a pre prepared standard graph to
determine amount present.
procedures
1) Prepare a standard curve for a range of known concentrations by
ƒ Preparing standard solutions over the range of 1 to 8% KCl by adding
the appropriate amount of standard potassium chloride solution (0.5
ml = 1%, the equivalent of 3.5 lb/bbl or 9.99 kg/m3) to centrifuge
tubes and diluting to the 7cc mark with distilled water.
ƒ Adding 3 cc’s of Sodium Perchlorate solution to each tube.
ƒ Centrifuging for one minute at approximately 1800 revs. With the hand
crank centrifuges normally provided offshore some practice will be
required to ensure consistency from test to test.
ƒ Plotting mls of precipitate against lb/bbl (kg/m3) of potassium chloride
using rectangular graph paper. Obviously this procedure will only need
to be done once at the commencement of drilling.
Example of KCl Concentration Standard Curve
Example of KCl Concentration Standard Curve
1.6
1.4
1.2
Millilitres of Precipitate
0.8
0.6
0.4
0.2
0
0 1 2 3 4 5 6 7 8 9
% KCl
26
2) Measure 7 mls of filtrate into the centrifuge tube.
3) Add 3 mls of Sodium Perchlorate solution.
4) Centrifuge for one minute at approximately 1800 revs.
5) Read the precipitate volume immediately.
calculations
Determine the potassium chloride concentration by comparing to the,
previously prepared, standard graph.
interpretation
As potassium ion – direct reading above
mbt test
discussion
The cation exchange capacity (CEC) is a measure of the potential reactivity
of the clay components of mud solids or shales. Clay minerals all exhibit ion
exchange behaviour to some degree. Isomorphous substitution of various
cations onto a clay surface depends on the number of available exchange
sites per unit weight of solids, reported in lb/bbl bentonite equivalent or
meq/100 g.
Cation exchange capacities in clay minerals are not a very precise or

fundamental quantity, as it varies significantly with pH. Some reported CEC’s
are as follows;
Vermiculites 120 - 200 meq/100g

Smectites 80 - 150 meq/100g
Illites 10 - 40 meq/100g
Kaolinite 1 -10 meq/100g
80 % of all sedimentary rocks are shales, which are generally composed of

varying proportions of these clay minerals. The CEC of shales can generally
be classed as follows;
Non-dispersive 0 - 10 meq/100g
Moderate dispersion 10 - 20 meq/100g
Dispersive 20 - 30 meq/100g
Highly dispersive > 30meq/100g
Increasing MBT values indicate both an increases in solids content, (whether

clay or no), and/ or a decreases in particle size distribution. Both of these
conditions are undesirable as ultimately they lead to deterioration in mud
properties and a consequent increase in mud costs.
The test is one of the key triggers for dump and dilute treatments and so due
care and attention must be given to the procedures and the interpretation of
the results.
An upper limit for MBT values will be given in the mud program and this
reflects a level above which, experience has shown, the efficiency of the
system is compromised.
27
Section
equipment
ƒ Methylene Blue Solution ( 3.74 USP grade)
ƒ 3% Hydrogen Peroxide
ƒ 5 N Sulphuric Acid
ƒ 125 ml Conical Flask
ƒ 25 ml Graduated Measuring Cylinder
ƒ Hot plate
ƒ Stirring Rod
ƒ Filter paper, Whatman No 4
ƒ 2 x 5ml Syringes
ƒ 0 ml Burette and clamp stand
procedures (mud solids)

1) Measure 2.0 mls of mud into the 125 ml conical flask.
2) Add 15 ml of the 3 % hydrogen peroxide using a measuring cylinder.
3) 1 ml of the 5 N Sulphuric acid using a clean syringe.
4) Swirl mixture gently to ensure mud solids are completely dispersed within
the mixture.
5) Place conical flask on a hotplate and heat gently until simmering. Leave
to simmer for about 10 minutes.
6) Dilute to approximately 50 ml with distilled water and stir.
7) Add 1ml increments of the methylene blue indicator via a burette and
swirl the flask vigorously for 30 seconds.
8) After each addition dip the end of the stirring rod into the solution and
apply a drop to the filter paper.
9) The end point is reached when the colour of the blue solids containing
droplet migrates away from the nucleus to form a light blue/turquoise
halo.
10) Once you reach the end point it is
important to keep stirring the mixture
and dropping further solution onto the
filter paper to ensure the end point is
persistent and has actually been reached.
Cation exchange is a time dependent
process and the solution will go on
reacting if all the sites have not been
completely exchanged.
calculations
Bentonite (equivalent) ppb = mls of methylene
blue solution X 2.5
procedure (shale)
1) Dry shale at 220 ˚F (104 ˚C) in an oven for 16 hours.
2) Grind shale using a pestle and mortar
3) Weigh 0.57 g of powdered shale into the conical flask and repeat steps
ii - xiii in the Mud Solids procedure above.
28
calculation
CEC (meq/100g) = mls of methylene blue solution x 1.95
This test, in association with the solids content, tells us something about the
type, size and therefore the active surface areas of solids in the mud.
interpretation
The result of this test could be the trigger for dump and dilute treatments
depending on the activity of the formations being drilled.
However in formations of low activity the low gravity solids content may
reach undesirable levels before the MBT reaches the programmed upper limit.
In this case the LGS content becomes the trigger point.
In cases where the LGS content remains low but the MBT reaches trigger point
whole mud dilution is the only solution – there is either a build up of highly
active clay or, more likely, a problem with ultrafines / colloidal material.
glycol – cloud point and % by vol

concentration
discussion
TAME (thermally activated micro emulsions) polyols are used primarily
to stabilise reactive clays and to minimise pressure transmission through
tectonically stressed shales.
In order to optimise the benefits of the clouding point mechanism of TAME

polyols, it is necessary to engineer the cloud point. For optimum performance
from cloud point polyols, the cloud point should be maintained close to, or
slightly lower than the BHCT (bottom hole circulating temperature).
Generally TAME polyols are effective at concentrations of 2 – 3% by volume of

the aqueous phase
Note: the percentage volume of polyol is always expressed as a percentage of

the aqueous phase and not of the whole mud.
Depletion of the polyol concentration while drilling is usually very low.

Consequently, the key to maintaining an adequate concentration in the
active mud system is to ensure that all new mud added to the active
system contains 3% by vol and any direct water additions, intentional or
unintentional, are compensated for by appropriate additions of glycol.
29
Section
equipment
ƒ Hot plate
ƒ 10 ml measuring cylinder
ƒ Thermometer – Mercury or Alcohol
procedure – cloud point

1) Collect at least 3 ml of filtrate in a 10 ml glass cylinder.
2) Put the 10 ml glass cylinder in a conical flask of water.
3) Heat up slowly on a hot plate.
4) Using either a mercury or alcohol thermometer take the temperature
of the filtrate as soon as it starts to become cloudy. This temperature is
called the cloud point.
calculations
Knowing the cloud point and the KCl concentration, derived from either
the potassium ion – direct reading or potassium ion – sodium perchlorate,
the polyol concentration can be obtained from empirically derived charts
showing polyol concentrations as a consequence of KCl concentration versus
cloud point temperature.
Where a blend of different cloud point polyols are being used, it is not
possible to determine the polyol concentration by the above method. In
these situations it is necessary to track the concentrations by the material
balance method.
interpretation
By increasing the concentration of either the KCl and/or the polyol the cloud
point can be lowered. Conversely by decreasing the concentration of either
the cloud point can be raised. By utilising this the cloud point can be
engineered for downhole temperatures in order to achieve optimum stability
when drilling reactive claystones or stressed shales.
Reliable BHCT can be obtained from the downhole measure while drilling
tools (eg. MWD or FEWD).
The cloud point, BHCT and polyol % by vol should be recorded on the daily
mud report as part of each full mud check.
garrett gas train - sulphides

discussion
The presence of hydrogen sulphide in a drilling fluid can be lethal to personnel
as well as being damaging to equipment and mud properties.
Hydrogen sulphide will dissolve in the fluid and remain in solution until
saturation point has been reached when it will break out.
It is very important to know if H2S is entering the fluid and it is obviously

advantageous to detect it before it is picked up by gas detectors, after having
broken out on surface.
30
The presence of hydrogen sulphide in the mud manifests itself in two ways as
it goes into solution. Firstly there will be a rapid drop in the pH as hydrogen
ions are neutralised. Secondly soluble sulphides will appear in the mud.
Measuring the latter of these two will provide conclusive evidence of hydrogen
sulphide in the mud.
Active soluble sulphides can be analysed and monitored because of their

characteristic reaction with acid that involves the release of H2S gas.
The test is performed on mud filtrate.
equipment
ƒ Garrett Gas Train: consisting of a transparent plastic gas train, an inert gas
supply (CO2N2 or N2O) with pressure regulator, a floating ball flowmeter
and a Dräger tube.
ƒ Flexible tubing.
Syringe to inject
Dispersion Dräger
Acid and Aktaflo E
Tube Tube
Injection Tube
Rubber Bung Exhaust
Gas Supply
Exhaust
1 2 3
Flowmeter
Porous China Magnetic Magnetic Mud
Membrane Stirrer Pellet Stirrer
ƒ Low and high range Dräger analysis tubes, the first marked `H2S 100/a´- CH
29101 and the second `H2S 0.2%/A´ - CH 28101. Ensure the Dräger tubes to
be used are within their use by date.
ƒ Dräger Multigas Detector Hand Operated Vacuum Pump, Model 31.
ƒ Stopcock: (2-way bore): 8 mm glass with Teflon plug.
ƒ Sulphuric Acid: 5N, reagent grade. Ensure
ƒ Hypodermic syringes: one 10 cc. (for acid), and one each 10 cc, 2.5 cc and Dräger tubes
1.0 cc (for sample). are within
their “use by
ƒ Hypodermic needles: two 1.5 inch (38 mm) with 21 gauge needles.
date
ƒ Octanol defoamer in a dropper bottle.
ƒ Inert Carrier Gas: Nitrogen (N2) bottle with low pressure regulator
(preferred), or Nitrous oxide (N20) cartridges.
ƒ Deionised water.
31
Section
procedure
1) With the regulator backed off install and puncture a CO2 cartridge in the
carrier gas assembly.
2) Add 20 ml of distilled water to chamber one.
3) Add 5 drops of Octanol to chamber one.
4) Add the required volume of mud filtrate into chamber 1 as determined
by which Dräger tube is to be employed and an estimate of the sulphide
range.
Sulphide Sample Dräger Factor

Range Volume Tube Tube
(mg/l)

1.5 - 30 10.0 ml H2S 100/a 12

3 - 60 5.0 ml “ 12

60 - 120 2.5 ml “ 12

60 - 1020 10.0 ml H2S 0.2%/a 600

120 - 2040 5.0 ml “ 600

240 - 4080 2.5 ml “ 600
5) Select a Dräger tube for the estimated range as per the table above and
break the tip from each end.
6) Install the tube with the arrow pointed down in the receptacle bored in
the corner of the train. Be sure the “O”-ring seals.
7) Install the clean, dry flow meter tube with the word TOP upward. Be
sure the “O”-ring seals.
8) Install the top on the gas train and hand tighten all screws evenly to
seal.
9) Attach the flexible tubing to the dispersion tube and to the Dräger
tube. Use only latex or flexible, inert plastic tubing. Do not clamp the
flexible – it does not require it and will provide pressure relief in the
event of over pressurisation.
10) Adjust the dispersion tube to 0.5 cm from bottom.
11) Put 10 ml of 5N Sulphuric acid into the hypodermic syringe.
12) Gently flow CO2 for 15 seconds to purge the system, checking for leaks.
Stop the flow.
13) Slowly inject the 10 ml of acid into chamber one through the rubber
septum.
14) Restart the carrier gas flow and adjust the flow so that the ball is between
the red lines. (200 to 400 cm3 per minute – one CO2 cartridge should
provide between 15 and 20 minutes of flow at this rate).
15) Continue flowing for a minimum of 15 minutes.
32
16) Observe changes in the appearance of the Dräger tube and record the
maximum darkened length, in units marked on the tube, before the front
starts to smear.
ƒ Any soluble sulphites in the fluid will, upon the addition of acid,
convert to sulphur dioxide (SO2) gas that can interfere with test
results.
ƒ In the low range tube this manifests itself as diffusion at the front
of the sulphide stain. The stain itself may be of a lighter colour than
when SO2 is not present and a lower reading may be attained.
ƒ It is important to note that while SO2 can produce a negative error it
does not falsely indicate a positive H2S reading.
ƒ In the high range tube an orange colour may appear ahead of the
black front if sulphites are present in the sample. The orange section
should be ignored when darkened length is recorded.
calculations
Using the sample volume, the Dräger tubes maximum darkened length and the
tube factor the sulphides present are calculated as:
darkened length x tube factor
Sulfides mg/l =
sample volume ml
For the higher range tube it may be necessary to correct the tube factor.
The tube factor is based on a batch factor (stencilled on the box) of 0.40.
If a different batch factor is stencilled on the box a corrected tube factor
should be calculated as follows:
Corrected tube factor = 600 x actual batch factor
0.40
interpretation
Any indication of soluble sulphides in the mud would indicate the
presence of H2S gas. With water based muds it is vital to remember that
H2S can be a by-product of degrading drilling fluid additives. Make sure
biodegradation is eliminated as a source of H2S before starting treatment
programs.
It may be the case however that the presence is due to the release of
gas from the pore spaces of the rock actually being drilled. In this case
ensuring proper overbalance and maintaining alkalinity is sufficient to
control any hazard.
This is not suitable for dealing with influxes, as the alkaline neutralisation
of H2S is instantly reversible by reductions in pH. In these cases a
scavenger, such as zinc oxide, should be added to convert soluble sulphides
into an insoluble precipitate, thus removing them permanently from the
equation.
Where H2S is expected it is advisable to pre-treat with a scavenger.

However with a scavenger in the system no indications of H2S will be
picked up, by conventional means, until the scavenger has been used up.
Thus while a scavenger increases safety levels it makes detection of small
amounts of H2S very difficult indeed.
33
Section
garrett gas train - carbonates

discussion
This method of quantifying the amount of soluble carbonate, bicarbonates
and carbon dioxide in the mud filtrate is far more accurate than the P f :M f
relationship.
Carbonate or bicarbonate contamination usually occurs as a result of CO2

influxes or over treatment with soda ash or sodium bicarbonate when
treating out cement contamination. They can also result as a consequence
of thermal degradation of organic compounds such as lignosulphonates and
lignites at temperatures >300 °F (148.9 °C). The final source of carbonates
can be contaminated Barite.
The test is based on converting all bicarbonates and carbonates to CO2,

which is then evolved by bubbling an inert carrier gas through the sample.
The gas stream is collected and subsequently drawn through a Dräger tube
at a fixed rate. The amount of total soluble carbonates is then calculated
based on the length of the purple stain in the Dräger tube.
The test is performed on mud filtrate.
equipment
ƒ Garrett Gas Train: consisting of a transparent plastic gas train, an inert
gas supply (N2 or N2O) with pressure regulator, a floating ball flowmeter
and a Dräger tube.
Garret Gas Train Setup for Measuring Carbonates

ƒ Flexible tubing: Type inert to carbon dioxide.
ƒ Dräger CO2 Analysis Tube: marked CO2 0.01 %/a - (No. CH-308-01).
ƒ Dräger One litre Alcotest Gas Bag: (No 7626425).
Ensure Dräger
ƒ Dräger Multigas Detector Hand Operated Vacuum Pump, Model 31.
tubes are within
ƒ Stopcock: (2-way bore): 8 mm glass with Teflon plug. their “use by
ƒ Sulphuric Acid: 5N, reagent grade. date”
ƒ Hypodermic syringes: one 10 cc. (for acid), and one each 10 cc, 2.5 cc and
1.0 cc (for sample).
ƒ Hypodermic needles: two 1.5 inch (38 mm) with 21 gauge needles.
ƒ Octanol defoamer in a dropper bottle.
ƒ Inert Carrier Gas: Nitrogen (N2) bottle with low pressure regulator
(preferred), or Nitrous oxide (N20) cartridges.
ƒ Deionised water.
Note: Nitrogen is preferred over nitrous oxide as the carrier gas. Because nitrous
oxide cools upon expansion and chills the diaphragm in the regulator,
prolonged flow will cause the regulator to perform erratically.
procedure
1) Be sure the GGT is clean, dry and on a level surface, with top removed.
2) Check bag and pump for leaks. To check the pump, insert a sealed
Dräger tube into the pump opening and depress bellows. It will remain
depressed if pump does not leak.
34
3) Add 20 ml of deionised water to chamber one.
4) Add 5 drops of Octanol to chamber one.
5) Install the top on the gas train and hand tighten evenly to seal all O-
rings.
6) Adjust the dispersion tube to approx 1/4” (5 mm) off bottom.
7) With regulator backed off, connect carrier gas supply to glass dispersion
tube of Chamber one using flexible tubing.
8) Flow carrier gas through train for one minute to purge air from the system.
Check for leaks in gas train unit.
9) With bag fully deflated install flexible tubing from stopcock bag onto the
outlet of chamber three.
10) Inject a measured volume of filtrate into chamber one through septum
with hypodermic syringe and needle. See table
Carbonate Sample Dräger Factor

Range Volume Tube Tube
(mg/l)

25 - 750 10.0 ml CO2 100/a 2.5

50 - 1500 5.0 ml “ 2.5

250 - 7500 2.5 ml “ 2.5
Note: For best Dräger tube accuracy, the stain length should fill more than half
the tube length, therefore sample volume must be carefully selected.
11) Slowly inject 10 ml sulphuric acid solution into chamber one through
rubber septum using a clean syringe and needle. Gently shake the gas
train to mix acid with sample in chamber one.
12) Open the stopcock on the gas bag. Restart gas flow and allow gas bag to
fill steadily during a 10 minute interval. When bag is firm to touch (do not
burst it!), shut off flow and close the stopcock.
13) Break the tip off each end of the Dräger tube.
14) Remove the tubing from chamber three outlet and reinstall it onto
the upstream end of the Dräger tube. Attach Dräger hand pump to
downstream end of Dräger tube.
15) Open the stopcock on the bag. With steady hand pressure, fully depress
the hand pump. Release pump so that gas flows out of the bag and
through the Dräger tube. Ten strokes should empty the bag. More than
ten strokes indicates leakage occurred and your results will not be
accurate.
16) Record the stain length in units marked on the Dräger tube (include the
faint blue tinge in the purple stain length reading).
17) To clean the GGT, remove the flexible tubing and remove the top.
Wash out the chambers with warm water and mild detergent using a
brush. Use a pipe cleaner to clean the passages between chambers.
Wash and rinse the unit with deionised water and allow to drain dry.
Be sure to periodically replace the disposal gas bag to avoid leaks and
contamination in the bag (bag replacement is suggested after 10
analyses).
35
Section
calculations
Using the sample volume, the Dräger tube’s stain length and the tube factor
the total soluble carbonates (CO2 + CO3– – + HCO3– ) present are calculated as
follows:
stainlength x tube factor
Carbonate mg/l =
sample volume ml
Reaction Amounts:
Lime: 0.00043 lb (.00123 kg/m3) treats 1.0 mg/l CO3– –
0.00021 lb (.0006 kg/m3) treats 1.0 mg/l HCO3–
interpretation
Excessive amounts of carbonates or bicarbonates can cause severe rheology
problems, particularly high and progressive gel strengths, and filtration
control problems. Typically these effects are worse in high solids muds in high
temperature applications. The symptoms are very similar to a build up of very
fine reactive solids. Care must be taken not to confuse the two very different
problems, as their solutions are completely different.
The acceptable concentration of carbonates will always depend on the

concentration of solids, temperature and chemical concentrations. Generally
a range of 1200 - 2400 mg/l is tolerated by most mud systems.
It is recommended that not all the carbonates be treated out. A minimum of

1000 - 1200 mg/l should be allowed to remain in the system.
The presence of carbon dioxide manifests itself in three ways as it goes into
solution. Firstly there will be a rapid drop in the pH. Secondly the ratio between
Pf and Mf will increase. Thirdly, depending on the pH, the Ca++ mg/l might
drop. However, the presence of calcium in the filtrate, as detected in the
Hardness titration does not eliminate the possibility of a carbonate problem.
Always pilot test the proposed solution before treating the active system for
carbonates.
The basic treatment for carbonate contamination is to precipitate the

carbonate with the calcium ion derived from Lime. However, the addition of
calcium will have no effect on bicarbonates. These first must be converted
to carbonates by addition of OH- ions. This is achieved by additions of
Lime. Bicarbonates cannot exist in the presence of hydroxyls. Under normal
conditions bicarbonates convert to carbonates at a pH above 9.5
Lime is slow to go into solution in most mud systems. This can be accelerated
by adding Lime, mixed in water, via a chemical barrel.
If necessary, Citric Acid can be added to limit the pH increase from Lime.
However, don’t prevent the bicarbonates from converting to carbonates by
lowering the pH too much, i.e. <9.5.
If PHPA is a component of the mud system the higher pH necessary to

treat out carbonate contamination will have an adverse effect on it. Fresh
additions of PHPA should be made to compensate once the contamination
has been treated out, the pH reduced to <9.5 and there is no chance of
further carbonate contamination.
36
silicate testing
the titration method
The procedure describes a method as per SPE 35059 to determine silicate
concentration in the drilling fluid. The procedure will also evaluate the
alkalinity (sodium content).
Silicates have an affinity with glass so the test may be carried out using plastic
titration dish. In case only glass beakers etc are available they need to be
washed very thoroughly after every test.
equipment
ƒ pH Meter with calomel electrode
ƒ Balance, accurate to 0.1g
ƒ Stirrer c/w small stir bar
ƒ Pipettes, 5 ml and 2 ml
ƒ Plastic titrating dish
ƒ De-ionised Water
ƒ Hydrochloric Acid, 0.2N
ƒ Hydrochloric Acid, 2.0N
ƒ Methyl Red Indicator Solution
ƒ Sodium Fluoride, reagent grade
ƒ pH buffers, pH 4 and 10
procedure
blank titration
A blank titration is first performed to compensate for Silica present in the
reagents.
1) Take 5 ml de-ionized water into the plastic titration dish and add 1 drop
of methyl red.
2) Add 0.2N hydrochloric acid until the colour first changes to pink.
3) Add 1g Sodium Fluoride. Stir the mixture. The colour changes to yellow.
4) Titrate with 2.0N Hydrochloric Acid to a pink colour change, at pH 6.0.
5) Record the amount of acid used -. A.
alkalinity (sodium content)

1) pH meter should be calibrated.
2) Take 5 ml of de-ionised water into a plastic titrating dish and add 1 drop of
methyl red indicator.
3) Set the beaker on a stirrer, and insert the pH electrode. The indicator
solution is used as a guide, but accurate measurements are against the
pH value.
4) Add a few drops of 0.2N Hydrochloric Acid, until the colour is pink.
5) Pipette 2 ml of filtrate into this beaker. The colour changes to yellow.
6) Titrate with 0.2N Hydrochloric Acid to pH 5.5, or when the colour will
change to pink note the volume of acid used (B).
silica (SiO2) content

1) Weigh 1 gm of Sodium Fluoride and add to the above titrated sample. The
colour will change to yellow, and the pH will rise to 8 - 9.
2) Titrate with 2.0N Hydrochloric Acid to pH 6.0, and record the volume of acid
used (C).
37
Section
calculation
alkalinity
For a 2 ml sample:
Na2O= 31,000 x A x N (mg/L)
V
K2O= 47,000 x A x N
V (mg/L)
Where:
A is ml of acid to first colour change
N is acid normality (0.2 N)
V is ml of filtrate sample
silica (SiO2)
For a 2 ml sample
ppm(mg/I)SiO2= 15000 x N x (C-A) SiO2= 15000 x N x (C-A) (mg/L)

2 (samplevol) V
g/I SiO2= 15 x N x (C-A)

2 (samplevol)
Where:
“C” is the volume of 2.0N Hydrochloric Acid used in the titration,
“A” is the volume of acid used in the blank correction (typically <0.1 ml),
“N” is the normality of the acid (2N).
To convert g/l SiO2 to % vol/vol Silicate in system
% vol Silicate = g/l SiO2 x 0.2237
Where the S.G. of Silicate is 1.475, with a SiO2 activity of 30.3% wt.
38

03-Section 3A WBM Testing

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03-Section 3A WBM Testing

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testing

mud testing procedures

section 3b - naf testing procedures

3 mud testing procedures

good laboratory practices

Keep the mud lab clean and tidy.

wbm testing procedures

3a wbm testing procedures

wbm testing procedures

procedure – standard balance

1) Follow steps 1 - 5 as for the standard mud balance procedure.

3a wbm testing procedures

The funnel viscosity will be measured in seconds per quart.

The funnel viscosity is, therefore, a more relevant indicator of trends in a

Instrument constants have been adjusted so that the Bingham plastic

The thermometer used must be calibrated against a mercury or alcohol

The rheometer readings may be taken at a higher temperature, to reflect flow

Note: Maximum operating temperature is

The gelling characteristics of the fluid can

3a wbm testing procedures

Plastic Viscosity (PV) in = 600 reading - 300 reading

Yield Point (YP)

Consistency Index (K):

YP in Ib/100 ft2 = (2 X 100 rpm reading) – 200 rpm reading

3a wbm testing procedures

It can be appreciated that a combination of all, or some of the factors

SG of mud in retort = SGm

This test is a reliable indication of the condition of a drilling fluid on a one

3a wbm testing procedures

However any change in fluid loss properties is a good indicator of general

Generally speaking, therefore, an increasing trend is bad and a decreasing trend

The thermometer used must be calibrated against a mercury or alcohol type

3a wbm testing procedures

3a wbm testing procedures

pH expresses acidity or alkalinity of an aqueous solution. An acid can be

The pH of a water based mud is controlled to improve the performance of

A balance is struck between these factors when choosing a pH for any

The recommended method for pH measurement is with a glass electrode

ƒ Distilled or deionised water: in spray bottle.

3a wbm testing procedures

procedures – pH indicator strips

filtrate alkalinity – Pf and Mf

Pf and Mf refer to titrations performed on the mud filtrate (f ). The P refers to

Hydroxyl ions Mud stable and in good condition

Knowledge of the mud and filtrate alkalinity is essential to ensure proper

3a wbm testing procedures

Carbonates and Bicarbonates are usually responsible when analysis shows

The inherent inaccuracy in the second end point determination makes

If Carbonate or Bicarbonate contamination is suspected it must be confirmed

Experience shows, however, that in low solids polymer muds an increasing

The focus should, therefore, be on observing changes in fluid loss and

filtrate hardness – Ca++ and Mg++

When EDTA (sodium salt of ethylene-diaminetetracetic acid) is added to

EDTA-Na + Ca++ + Mg++ ----> EDTA- Ca + EDTA- Mg + Na+

If huge sources of Magnesium are encountered then it is pointless trying

In situations where hydroxide additions have no effect on pH and free

** 1 ml of Masking agent should be added if soluble iron is suspected to

procedures – total hardness

3a wbm testing procedures

calculations – total hardness

Remember, in a properly maintained alkaline system where excess OH– ions

Control calcium hardness with suitable treatments.

Cl- + AgNO3 → AgCl (white precipitate) + NO3-