section 3b

naf testing procedures

section 3b Scomi Oiltools

mud density 2
funnel viscosity 4
rheology 4
hthp filtrate – temperatures up to 300 °F (148.9 °C) 7
retort analysis – oil base mud 11
sand content 12
electrical stability 13
lime content 14
water phase salinity 15
garrett gas train - sulfides 17
oil on cuttings measurements 20
Section

3b naf testing procedures

naf 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/
ft3, 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.

Have you
The mud test kit will contain both standard mud balances and a pressurised
checked the
Halliburton mud balance. Both types are calibrated by weighing distilled mud balance
water at 70 °F (21.1 °C) and obtaining a reading of 1.00 SG / 8.33 lb/gal. If this lately?
is not the case adjust the balance by adding or removing lead shot as
required.

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 tourly 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
breakout.
4) Replace cap and rotate until it is
firmly seated, ensuring some of
the mud is expelled through the Example of standard mud balance
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.

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 has been placed on the cup, with the check 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 a
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 an OBM will vary according to the temperature of the sample.
Differences of up to 0.03 SG are normal between ambient and flowline
temperatures of 65 °C.

Mud weights noted on the mud report will refer to both the density at the
flow line temperature and the density at ambient temperature when the
sample has cooled.

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.


Section

3b naf testing procedures

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.

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 sec/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 Marsh funnel
ƒ Graduated cup: one quart / litre
ƒ Stopwatch
ƒ Thermometer: 32 – 220 °F (0 – 104 °C)

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 of little significance in relation to SBM. This is due to
the fact that SBM thin with heat and the result is therefore very temperature
dependent. However, if temperature remains constant, the funnel viscosity
may indicate trends that require further investigation.

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
carry a label noting the date of the last calibration.


Drilling fluid is contained in the annular space between two concentric
cylinders. The outer cylinder or rotor sleeve is driven at a constant
rotational velocity. The rotation of the rotor sleeve in the fluid produces
a torque on the inner cylinder or bob, and the dial attached to the bob
indicates displacement of the bob. This is the standard procedure
recommended by API 13B for field testing oil 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. When checking oil
base mud systems
The six readings will be taken at 120 °F (48.9 °C). A heated cup will be used it is recommended
to insert the
for this purpose. Synthetic Base Muds exhibit thinning tendencies with
thermometer in
temperature and so it is still necessary to standardise this test by taking the the actual fluid to
readings at the same temperature on each occasion. ensure the correct
testing temperature
The thermometer used must be calibrated against a mercury or alcohol has been reached
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, only the 120 °F (48.9 °C) readings will be entered
in the mud check columns on the mud report. 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
if increasing rheology is becoming a problem a 30 min gel should also
be taken in order to determine the effectiveness of the treatment program.

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 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
Example of 6 Speed
reading has stabilised at this speed before noting
Rheometer
the result and proceeding to the 300, 200, 100, 6
and 3 RPM speeds.


Section

3b naf testing procedures

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.

calculations
Apparent Viscosity (AV) in = 600 reading ÷ 2
Centipoise (cps)
Plastic Viscosity (PV) in = 600 reading - 300 reading
Centipoise (cps)

Yield Point (YP):

Yield Point (YP) in lb/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 lb/ 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 lb/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.

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.

hthp filtrate – temperatures up to 300 ˚F (148.9 °C)

discussion
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 utilised 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.

This test provides the definitive rigsite answer, (more sophisticated

equipment is available in onshore laboratories), to the effectiveness of the
emulsification package and the quality of the filter cake.

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

ƒ HTHP Filtration Cell - Diameter 3” x Height 3.0”

ƒ OFI specially Hardened Filter paper - Diameter 2.5” / Filtration Area 4.91
sq.in
ƒ High Pressure CO2 supply (600 psi - 4138 kPa)
ƒ Stop Clock
ƒ 10 and 25 ml measuring cylinders


Section

3b naf testing procedures

procedure
1) To standardise this test the following procedure must
be adhered to. Backpressure is applied during the test
to avoid filtrate evaporation.
2) Allow the heating jacket to reach the required
temperature.
3) 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 dirt.
4) Tighten the bottom valve stem, taking care not to over
tighten, and fill the cell to about 0.5 inch from the rim. Example of HTHP
5) Place a filter paper on the rim and put the lid on the cell. Filter Press
Ensure the lid stem is open while doing this to avoid
damaging the filter paper.
6) Tighten the six studs in the bomb and close the lid stem.
7) Place the bomb in the heating jacket with the lid facing downwards.
Rotate the bomb until it seats on the locking pin.
8) Place a CO2 cartridge in each regulator and tighten up the retainers.
9) Place the top regulator on the stem and engage the locking pin. Close
the bleed off valve and turn the regulator clockwise until 100 psi Do not use nitrous oxide
(690 kPa) is showing on the gauge. (N2O) as a pressure
10) Repeat the process with the bottom regulator. source for this test. N2O
11) Turn the top valve stem 1/4 to 1/2 turn anti clockwise to pressure up the can detonate when
under temperature and
cell to 100 psi (690 kPa).
pressure in the presence
12) When the cell reaches the required test temperature open the bottom of oil, grease, or
stem (1/2 turn) and then increase the pressure on the top regulator to carbonaceous materials.
600 psi (4138 kPa) over +/- 20 seconds. Use only carbon dioxide
13) Commence the test. The test should be carried out as soon as the (CO2) or nitrogen (N2).
bomb reaches the test temperature. Leaving the cell for long periods at
high temperatures will produce unreliable results.
14) If the pressure on the bottom regulator increases significantly above
100 psi (690 kPa) bleed off some of the filtrate into the graduated
cylinder.
15) After 30 minutes, close the top and bottom valve stems. Slack off
the regulator on the bottom collection vessel. Bleed off the filtrate into
the graduated cylinder. Disconnect bottom collection vessel, fully
open the bleed off valve and tip any residual filtrate into the graduated
cylinder. If the bottom
16) Bleed the pressure off the top regulator. pressure rises 20 psi
17) Disconnect the top regulator and remove the bomb from the heating above the specified
jacket, allowing it to cool in a safe place. pressure during
the test, carefully
18) When the bomb has cooled bleed off the trapped pressure by
bleed off pressure
slowly opening the top valve with the bomb in an upright position. by draining a small
With the residual pressure bled off invert the cell, loosen the six studs volume of filtrate.
and remove the lid.
19) Examine the filter paper and report the thickness in 32nds (mm) of
an inch. Comments about the quality of the cake should be noted in the
comments section of the mud report i.e. tough rubbery etc.


20) Thoroughly clean the bomb and stems in preparation for the next test.
21) Do not preheat the bomb by resting on the heating jacket.

calculations
The total filtrate volume, both oil and water, should be doubled, as the
standard API press is twice the area of the HPHT cell. Record the volume
of water, if any, in the filtrate and remember that this volume must also be
doubled for reporting purposes.

interpretation
There should be no free water in the filtrate – any indication of water would
indicate a problem with the emulsification package that requires immediate
attention.

The oil fraction should be clear with no hint of muddiness. If there is any sign
of mud in the filtrate then the result of the test is void.

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.

retort analysis – oil base mud

discussion
The accurate determination of the oil, water, high gravity solids and low
gravity solids in an OBM mud relies on the correct usage of the 50 ml retort and
the correct interpretation of the results.

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 the oil phase. The heavy fraction can easily account
for up to 1% of the total volume and a failure to distil this will result in an
equivalent increase in apparent solids content.

It is critical that the correct mud weight is used in the calculation to determine
the relative concentrations of HGS and LGS. It is commonly the case that
the difference in density between a hot and cold OBM is .03 sg. 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.


Section

3b naf testing procedures

The volume of the retort will be confirmed by filling the cell with distilled
water 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.

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 trof
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 Example of Retort
change the steel wool can result in inaccurate
measurements, as this extraneous water will
become included in the total water content.

10
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 and the final drops coming out of
the retort should be observed to be black (the heavy fraction) and sink
through the clear oil to the meniscus. Ultimately smoke will emerge from
the retort and the distillation is only complete when the smoke stops.

calculations
It will be assumed that all salt in the brine phase is Calcium Chloride.

SG of drilled solids (LGS) = 2.60

SG of Barite (HGS) = 4.25
SG of Base Oil = SGo

Input Data

SG of mud in retort = SGm

Retort % oil = Of
Retort % water = Wf
Retort % solids = Sf

mls of 0.282N AgNO3 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 =
CS
Solids (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

11
Section

3b naf testing procedures

= %LGS x 9.1
lb/bbl HGS = %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 OBM 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.

It is possible to envisage a situation where vast sums of money are spent

treating a non-existent solids problem.

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 HTHP 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.

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” 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 glass measuring tube to the indicated
with mud. Add clean base oil to the next
mark. Close the mouth of the tube and shake
vigorously.

Example of Sand Content

12
2) Pour the mixture onto the screen, add more base oil to the tube, shake
and again pour onto the screen. Repeat until the wash fluid is clear.
3) Wash the sand retained on the screen with base oil to remove any
remaining mud.
4) Fit the funnel over the top of the sieve. Invert slowly and insert the
mouth of the funnel into the glass tube. Wash the sand into the tube with
clean base oil.

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 powder. 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.

electrical stability
discussion
ƒ The test will be carried out at 120 °F
(48.9 °C) or whatever the rheology
temperature is carried out at. The mud to
be tested will be the mud in the heated
cup after the rheology measurements
have been completed.
ƒ Regularly check the accuracy of the ES meter with standard resistors
and / or Zener diodes The ES readings should fall within 2.5% of the
expected values; if any of the ES readings fall outside this range, the
instrument should be replaced.

equipment
ƒ The electrical stability will be measured with a Fann or OFI digital meter
and reported in volts.

13
Section

3b naf testing procedures

procedures
1) Before placing the probe in the mud, it is essential to test the meter in
air. The reading should go off scale and the display start flashing. If the
meter does not go off scale, it is an indication that the probe is shorting
out due to an accumulation of detritus between the two prongs. It is
clear that the probe can short out before the end point of the mud
is reached and an erroneous reading will result. The probe should be
carefully cleaned and retested in air to ensure that it now goes off scale
before testing the mud.
2) Place the clean and checked probe in the sample at 120 °F (48.9 °C)
and use it to stir the fluid to ensure homogeneity. Position the probe so it
does not touch the bottom or sides of the heated cup, ensuring the tip of
the electrode is completely immersed.
3) Press the button to initiate the voltage ramp, holding the probe still until
the end point is reached and a steady reading is seen in the digital display.
Note the reading.
4) Repeat the test. The two ES values should be within 5% and anything
greater would indicate a problem with the equipment.
5) The result is the average of the two readings.

calculations
The result is simply the average of the two readings in volts.

interpretation
It is essential to remember that the stability reading is not just a measurement
of emulsion strength and will vary with water percentage and water phase
salinity.

Trends are of more interest than absolute values. A decreasing stability

reading while other mud properties remained constant would be an
indication of decreasing emulsifier effectiveness.

lime content
discussion
The measurement of lime in the mud has been the subject of numerous
studies to establish why results often do not match known concentrations.
For example, a brand new mud mixed at the mud plant has 6 lb/bbl
(17.1 kg/m3) of lime added and yet the test may indicate only 3 lb/bbl
(8.55 kg/m3). Results will also be affected by the combination of contaminants
into the mud system. Magnesium will actually react with the OH ions in the
conical flask as water is added to the demulsified sample during the test and,
thus, no pink colour will develop when phenolphthalein is added.

It should be remembered that this test is measuring the pH of the sample,

as excess lime is dissolve d by the addition of distilled water.

The back titration method has been found to give the most accurate
measurement of the excess lime content of an OBM.

14
equipment
ƒ Xylene / Isopropanol (1:1 mixture) or equivalent
ƒ 250 ml conical flask
ƒ Variable temperature and speed hot plate/stirrer with suitable magnetic
beads
ƒ Distilled water
ƒ Phenolphthalein indicator
ƒ 0.1N H2SO4
ƒ 0.1N NaOH
ƒ Pipettes

procedures
1) Measure 50 ml of Xylene / Isopropanol (1:1 mixture) into a 250 ml conical
flask.
2) Disperse 1 ml of whole mud into the 50 ml of solvent while mixing on a
magnetic stirrer for 30 seconds.
3) Add 100 mls of distilled water, 10 drops of phenolphthalein indicator and
allow to mix for 5 mins. A strong pink / red colour will develop.
4) Add 10 cc’s of 0.1N H2SO4 - the red colour will disappear.
5) Back titrate with 0.1N NaOH until a pink tinge returns.

calculations
Alkalinity (Mp) = 10 - ml of NaOH
lb/bbl excess lime = Mp x 1.295
kg/m3 excess lime = Mp x (1.295 x 6.2897) ÷ 2.205
= Mp x 3.69

interpretation
It is important to maintain the lime content as recommended in the mud
program to optimise the emulsification package. Mud companies are often
of the opinion that lime is not required in modern emulsification packages.
However, experience has consistently shown that many mud problems
(thick mud, water in the filtrate etc) can be corrected by restoring a depleted
lime content.

If it is obvious that large lime additions to the mud are not being reflected
in test results then increasingly large amounts of lime should not be
continuously added – a masking agent is undoubtedly at work.

water phase salinity

discussion
Numerous papers have been generated explaining different ways of
reporting salinity eg ppm CaCl2 whole mud, mg/l Cl brine phase 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 is always reported as mg/l chlorides in the water

phase i.e. WPS.

15
Section

3b naf testing procedures

Remember ppm is not the same as mg/l (ppm x brine SG = mg/l)

It will always be assumed that all chlorides in the mud are from Calcium
Chloride i.e. there is no requirement to differentiate between Sodium Chloride
and Calcium Chloride.

equipment
ƒ Xylene / Isopropanol (1:1 mixture)
ƒ 250 ml conical flask
ƒ Variable temperature and speed hot plate/stirrer with suitable magnetic
beads
ƒ Distilled water
ƒ Potassium chromate indicator
ƒ 0.1N H2SO4
ƒ 0.282 AgNO3.
ƒ Pipettes

procedure
1) The chloride titration is a continuation of the lime content test.
2) Add 0.5 ml of 0.1N H2SO4 to remove the pink tinge from the sample
remaining from the lime test (more if required).
3) Add 15 drops of potassium chromate indicator to the colourless sample.
4) While agitating vigorously with the magnetic stirrer, titrate with 0.282
AgNO3.
5) The end point is reached at the first sign of a lasting orange tinge (not
brick red).
6) A heavy precipitate of silver chloride will develop during this titration.
To ensure even distribution of the AgNO3 the magnetic stirrer should
be at a high speed. However, not so high that the sides of the flask
become splashed with sample.

calculations
mls of 0.282N AgNO3 x 10,000
WPS mg/l =
% Water÷100

The result will be reported in mg/l of total Chlorides in the water phase.

interpretation
The accurate calculation of the WPS is obviously dependent on the precise
determination of the water content of the whole mud.

The end point must be consistently picked at the same colour change.

Great care must be taken to ensure that results are consistent over several
samples before embarking on a treatment program to increase salinity
levels. This is because while it is very easy to add salt, large dilutions with
freshwater, base oil and chemicals would be required to reduce the effects of
any over treatment.

16
garrett gas train - sulfides
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.

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 lime content
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.

Since the test is performed on whole mud, strong acids, such as sulphuric
acid, are not used since they would release inert sulphides (from barite for
example) which are non hazardous in normal drilling situations.

By adding citric acid, a relatively mild acid, to a whole mud sample in a

Garret Gas Train it is possible to detect the presence of active sulphides in
the mud.

equipment
ƒ A Garret Gas Train (GGT) – See detailed diagram.
ƒ The GGT separates the gas from the liquid, thereby preventing
contamination of the H2S detector by the liquid phase.
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.
ƒ The two types of Dräger tube will span a sufficiently wide range for
sulphide analysis of muds. The low range tube is white until H2S turns
it brownish black and the high range blue until turned jet black. No
other common mud contaminant or component has this affect.
ƒ Citric acid + demulsifier solution. This is prepared by dissolving 420
grams of reagent grade citric acid into 100 ml of deionised water and
stirring in 25 ml of Aktaflo E.
ƒ Octanol in a dropper bottle as a defoamer.
ƒ A 20 ml hypodermic syringe, with 21 gauge needle, for acid and a
selection of 2.5 ml, 5 ml and 10 ml disposable syringes for oil mud sample
volume measurements.
ƒ Magnetic stirrer with plastic or glass covered stirring bar to fit into
GGT chamber 1.

17
Section

3b naf testing procedures

procedure
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

1) Arrange the magnetic stirrer and GGT body so that the stir bar will rotate
freely to agitate the contents of chamber 1.
2) With the regulator backed off install and puncture a CO2 cartridge in the
carrier gas assembly.
3) Add the required volume of mud into chamber 1 as determined by which
Dräger tube is to be employed and an estimate of the sulphide range
(Chambers 2 and 3 remain empty as foam traps).

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

4) Select a Dräger tube for the estimated range as per the table above
and break the tip from each end.
5) Add 10 drops of Octanol to chamber 1.
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.

18
10) Adjust the dispersion tube to 0.5 cm from bottom or enough to clear
the stirring bar.
11) Put 20 ml of acid / Aktaflo E into the hypodermic syringe.
12) Gently flow CO2 for 15 seconds to purge the system, checking for leaks.
Stop the flow.
13) Start rapid stirring of the contents of chamber 1 while slowly injecting
the acid / Aktaflo through the rubber septum. Stir for at least 5 minutes
or until the sample is well dispersed with no obvious oil drops.
14) Restart the carrier gas flow and adjust the flow so that the ball is
between the red lines. (200 - 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.
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.
17) Thoroughly clean the unit after use.

calculations
Using the sample volume, the Dräger tubes maximum darkened length and
the tube factor the sulphides present are calculated as:

darkenedlength x tube factor

Sulfidesmg/I =
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:
actual batch factor
Corrected tube factor = 600 x
0.40

interpretation
Any indication of soluble sulphides in the mud would indicate the presence of
H2S gas. 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.

19
Section

3b naf testing procedures

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.

oil on cuttings measurements

introduction
When drilling with an SBM every effort must be made to minimise losses to
the sea.

The main source of SBM discharge is the shale shakers and is a consequence
of the SBM adhering to the cuttings that are discharged overboard.

A second source of fluid loss is through the centrifuges, once again as a result
of SBM adhering to the solids content.

There are two ways of measuring the amount of oil being discharged to the
sea.

ƒ Analyses of the amount of oil adhering to the cuttings and centrifuged

solids at any given time.
ƒ Analysis of the total amount of oil that has been lost to the sea at the
end of the well. This is a mass balance calculation based on the actual
amount of whole mud discharged during drilling operations.

The first method gives a snapshot of what is happening at the time the
sample is taken and does not really reflect the overall picture. The second
method gives a true measurement of what has actually been lost.

Typical target for Oil on Cuttings analysis is:

ƒ Less than 10% oil by weight (Both shakers and Centrifuges) (i.e. less than
100 grams of oil per kilogram of dry cuttings)

The primary variable in determining the percentage of mud associated with

the discharged rock is the size of the cuttings i.e. the larger the cuttings
the smaller the surface area, available for adhesion, for a given volume of
drilled formation. The converse is also true i.e. the smaller the cuttings the
larger the surface area. Other variables include shaker screen size, type of
formation, OWR and rheology.

If available, drying screens should be utilised in an attempt to reduce

the measured Oil on Cuttings (OOC) content to less than 10% by weight.
However this goal should not take preference over utilising the finest
possible screens on the shakers and maintaining the optimum mud
properties for drilling.

OOC analysis should be carried out at least once during every 24 hour
period when drilling has occurred. Testing will be more frequent during
periods of high ROP when a check should be performed at least every 300m
drilled.

20
Centrifuges should be run at such bowl speeds and flow rates as to ensure
the measured OOC is always less than 10% by weight. A check will be
performed, as per the shaker analysis, once in any 24-hour period the
centrifuges have been run.

oil on cuttings analysis

It is important that the weighted average OOC is reported along with
individual daily test results. This is reported as an expression of the percentage
of total cumulated oil discharge of the total cumulated cuttings discharge,
calculated daily.

This is because during periods of slower drilling the OOC is invariably

higher as more fines are generated. However long periods of slow drilling
will result in many days of high oil on cuttings results but not many feet/
meters being drilled – this arithmetical average is obviously, therefore a
distortion of the well average.

sampling
1) A representative bulk sample of at least 0.5 kg - 1.0 kg should be taken
and must include material from each deck of all the shakers. This is best
achieved by “scanning” a suitable container, preferably a wide tray which
will retain all the material i.e. both the solids and liquids, beneath the
discharge of the shakers.
2) The sample would then be thoroughly mulched to ensure a homogenous
sample.
3) Immediately transfer the sample to the mud lab for analysis.

equipment
ƒ Proprietary mud, oil and water retort kit with at least three mud chambers.
A 50 ml chamber must be used.
ƒ The distillate receiver must be an accurately calibrated 20 ml or 50 ml
measuring cylinder calibrated in 1.0 ml divisions (dependent on amount
of distillate expected).
ƒ A triple beam balance capable of weighing to an accuracy 0.1 g under
offshore conditions.

procedure
1) Weigh the distillate receiver.
2) Weigh the empty retort cell (top and bottom screwed together with
both the lid in place and the steel wool in the upper chamber).
3) Unscrew the retort and fill the bottom part with cuttings as completely as
possible, replace the lid and clean off any adhering mud and oil. Re-screw
the upper chamber.
4) Re-weigh the filled assembly.
5) Retort the sample for as long as it takes to burn off all the heavy fractions
of oil.
6) Switch off the heater, remove the mud chamber and allow to cool. Read
off the volume of the water and oil collected in the distillate receiver.
Reweigh the distillate receiver. Reweigh the retort assembly when it has
cooled.

21
Section

3b naf testing procedures

calculation
The result is calculated by the steps:

A = Weight of chamber (empty with steel wool + lid) gm

B = Weight of chamber and sample gm
C = Weight of empty graduated glass cylinder gm
D = Weight of chamber after heating gm
E = Weight of glass cylinder and distillate gm
F = Volume of distillate mls
G = Volume of water mls
H = Weight of cuttings (B - A) gm
I = Weight of dry solids (D - A) gm
J = Weight of distillate (E - C) gm
K = Weight of oil in distillate (J - G) gm
L = Volume of oil in distillate (F - G) mls

M = Calculate oil on cuttings (K ÷ I) x 1000 gm /

kg

Percentage oil on cuttings (M x 100) ÷ 1000 %

The content of oil in the cuttings should be expressed as grams of oil per
kilogram of dry retorted solids and in % by weight.

Mistakes have been made due to experimental error eg, the weight of
the dry solids plus oil and water does not tally with the weight wet cuttings
etc. The reporting form is designed to allow easy cross checks at a glance
and so ensure no erroneous results are taken as true.
ƒ The weight of wet cuttings (H) should be slightly more than the weight
of dry cuttings (I) + the weight of distillate (J). A slight amount of distillate
would appear to evaporate.
ƒ The weight of oil in the distillate (K) should equal the volume of oil (L) x
the SG of the oil.
It all sounds obvious but often these basic sums do not tally. If these simple
crosschecks reveal experimental error then the figures need to be checked
or the test repeated.

check calibration
The heating element in the retort kit can decline in efficiency over a period
of time and this needs to be checked. Such checks should be carried out,
for each well drilled with oil based mud:

ƒ Prior to drilling with OBM.

ƒ At completion of the well.

22
To calibrate a retort the following mixture should be mixed on a Hamilton
Beach mixer at the very high speed setting, adding each component in order
as listed below:

Base Oil 106 mls

Organophilic Clay 1.0 g
Emulsifier 3.0 mls
Lime 2.0 g
Fresh Water 28 mls
Wetting Agent 3.0 g
Barite 750 g

Mixing Notes:
ƒ The Barite should be added in stages, until the mixer can no longer
incorporate the solids (approximately 650 gm), the remaining Barite
should be thoroughly mixed in with a spatula.
ƒ The final mixture should be of a highly viscous, grainy-looking, semi-
solid nature, but fluid enough to allow proper filling of the retort cup.
ƒ The above mixture should yield a measured oil/water ratio of 80/20.
Solids content is 56%.
ƒ Total volume of the mix is 320 mls and thus one mix should be sufficient
for calibration of a 50 mls retort six times (allowing for the inevitable
losses).

The measured figure of oil on dry retorted solids should be within +/- 10
g/kg of the calculated value.

23