Ministry of Higher Education and

Scientific Research
University of Technology
Petroleum Technology Department
Scientific
Report

Pilot Test

Homam Mohammad Radhy

‫همام محمد راضي علوان‬
3rd Stage Morning
Drilling Fluid
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Pilot Testing

Homam M. Radhy A.
September/2020
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CONTENTS
1. Abstract …………………………………………………………………………. 3
2. Introduction ………………………………………….................……………….. 3
3. Designing Pilot Tests ……………………………………………………………. 4
4. Pilot Testing Equipment ……………………………………………………...… 5
5. Interpretation of Pilot Test Results ………………………………………..…… 5
6. Testing for Tracer …………………………………………………………..…… 7
References ………………………………………………………….…………… 11
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1. Abstract
The drilling fluid specialist uses the API diagnostic to detect potential problems and
identify their cause Alternative mud treatments then must be evaluated using small
samples This ensures that the mixture used will provide the desired results at the lowest
possible cost before treatment of the active mud system is started The units of measure
most commonly used when treating the active drilling fluid system are pounds for
weight and barrels for volume The units of measure most commonly used for pilot tests
are grams for weight and cubic centimeters for volume.

2. Introduction
Pilot testing of drilling fluids is testing performed on proportionately small-scale
samples. It is an essential part of drilling fluid testing and treating. Pilot testing
minimizes the risk of sending a fluid downhole that may be incompatible with the
formations to be drilled or that may be ineffective under downhole conditions.
Generally, pilot testing is concentrated on the physical properties such as rheology and
fluid loss; however, it is important that chemical properties also be evaluated. Most
chemical reactions require heat, mixing, and time to drive the reaction. Therefore, it is
necessary to have a means for heating and agitating pilot test samples. Problems such
as carbonates and bicarbonates are not readily detectable and require a complete mud
analysis and a pilot test series with heat aging to determine proper treatment. Without
heat aging, it is easy to overtreat the contaminant and create an even more severe
problem. A portable roller oven is a critical part of a pilot testing set-up at the rigsite.
A pilot test sample should be re presentative of the fluid being used. Pilot testing is thus
based on the fact that 1 g/350 cm3 of the sample is equivalent to 1 lb/bbl (42 gal) of the
actual mud system. (See Figure 1 which illustrates pilot testing equivalents.)

Figure 1
Pilot Testing Equivalents
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3. Designing Pilot Tests

A pilot test or a series of pilot tests must be designed to answer the questions that you
have in mind. Therefore, it is necessary to know exactly the reason for the test. Some
typical reasons are:
1. Mud response to downhole conditions, such as:
a. temperature effects
b. drilling uncured cement
c. drilling anhydrite
d. encountering salt/saltwater flows
e. acid gas (CO2, H2S) intrusions
f. water on water-based mud contamination in oil-based mud

2. Product response as a result of:

a. purity, material variation (different lot #s)
b. concentration
c. compatibility with other components in the mud
d. comparison to other products
e. temperature/contamination
f. shelf life

3. Adjustments to mud properties such as:

a. weight up/dilution
b. changing fluid loss properties
c. changing alkalinity/pH
d. treating carbonate/bicarbonate contamination
e. reducing hardness
f. adjusting MBT - clay content of the mud
g. changing oil/water ratio of oil muds
h. increasing electrical stability of oil muds

4. Study of effects of breakover, converting or displacement of muds, such as:

a. displacing water-based mud with oil-based mud or vice versa
b. converting from freshwater mud to saturated salt mud
c. breakover to lime or gyp mud
d. reducing components in mud to convert to bland coring fluid
e. treatment required to convert mud to a packer fluid

To determine how to design a pilot test or test series, look at economics and potential
for problems down the road. For example, if you expect to encounter a pressured
saltwater flow (16 lb/gal) with a 15 lb/gal freshwater mud at 350×F, the parameters for
testing could be: (1) maximum volume of saltwater anticipated in the mud, (2) weight
up to 16 lb/gal with and without contaminant, (3) effects of temperature on mud (15
and 16 lb/gal) with and without contamination, and (4) dilution and thinner treatments.
Pilot test design requires calculating amounts of materials to put into the test samples.In
pilot tests, grams are equivalent to pounds and 350 cm3 is equivalent to one 42-gal
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oilfield barrel. Material balance equations, as developed in “Engineering”, are used for
pilot test design. For example, to weight the 15 lb/gal mud to 16 lb/gal without
increasing the mud volume, one must calculate how much 15 lb/gal mud to dump and
how much barite to add to increase density. For simpler pilot tests, such as adding only
a few lb/bbl treatment, it is not necessary to account for material balance.

Rigsite pilot tests have distinct practical advantages over sending a mud into the
laboratory or having a laboratory mud prepared for pilot testing. Rigsite testing allows
actual material and mud to be used, which allows results to be readily available. quicker
(which is usually very important), and allows rig supervisor and mud engineer to
evaluate and review the pilot test results. Laboratory pilot tests and planning are both
important in preparing to drill a troublesome well. Both should be done long in advance
of anticipated problems. In this case, lab pilot tests are advantageous in that they can be
performed in advance, but then pilot tested again at the rigsite with the actual mud and
chemicals.

4. Pilot Testing Equipment

A balance that can weight from 0.1 to 300 g and an oven (preferably roller oven) that
can go to approximately 400×F are needed. Mud cells (three minimum) made of
stainless steel to hold at least 300 cm3 of mud at 1000 psi, a mixer such as a Hamilton
Beach mixer are also needed. Mud testing equipment that is accurately calibrated,
along with fresh reagents for titrations are essential for pilot testing. Most mud
companies can provide a Pilot Test Kit; they do not usually contain the oven and cells,
but are available upon request.

5. Interpretation of Pilot Test Results

A single pilot test can give only limited information, but this is often sufficient for the
need. Most often a series of pilot tests (three to five samples) are required to properly
answer the questions. For every pilot test (single or series) a control sample must be
run along in parallel w ith the test sample. A control sample is the base mud which has
not been treated, but which is taken through all the mixing, heating, rolling, etc.
processes. The control is used to aid interpretation of results. Data are compared
between the control and test sample to sort out the effects due to treatment versus
mechanical effects (mixing, rolling or time of exposure). For example, a mud engineer
has an oil mud with a low electrical stability (ES). He pilot tests a sample with 2 lb/bbl
(2 g/350 cm3) additional emulsifier and shears it on the mixer for 10 minutes. The ES
is much higher than before. He also has run a control sample on the mixer for 10
minutes, but without the additional emulsifier, and obtained almost the same higher ES.
Was the emulsifier responsible for the improved ES? No, in this case the shearing was
what gave the improvement.
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Results of pilot testing should be thoroughly reviewed before drawing conclusions.

Often, a pilot will lead to another one or two tests before the answer is satisfactorily
clear.
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6. Testing for Tracer

6.1 Calcium Carbonate Determination in Whole Mud
1. Put approximately 40 cc’s of de-ionized (or distilled) water and a magnetic
stirring bar into a 400-ml beaker, and place the beaker on a stir plate.
2. Precisely measure 10 cc’s of whole mud into the beaker while stirring. A large
syringe may be the easiest measuring device. (If measuring with a graduated
cylinder, or similar measuring device, rinse all of the mud into the beaker with
de-ionized or distilled water.)
3. While stirring, carefully add 25 cc’s of 15% HCl (hydrochloric acid) to the
beaker (the mud logger will have some). The HCl will dissolve the calcium
carbonate. Be sure to add the acid very slowly at first to prevent the resulting
effervescence from becoming uncontrollable. Stir the solution for at least 5
minutes.
4. Pour the solution in to a 200-ml volumetric flask. Rinse the beaker with de-
ionized or distilled water and add this liquid to the flask. Continue until all of
the material has been rinsed into the flask, and then add enough water to bring
the total in the flask exactly to the 200-ml mark. Cap the flask and shake the
solution to be sure it is homogeneous.
5. Transfer exactly 2 cc’s of solution from the flask into a titrating dish. Add a stir
bar. Add 2 cc’s of 1.0N NaOH and a pinch of Calver II indicator.
6. While stirring, titrate from wine color to blue with Versenate Hardness Titrating
Solution (1 ml=20 epm Ca).
7. Calculate the ppb of calcium carbonate in the mud as follows:
(CC’s titrating solution) x (3.5) = ppb calcium carbonate
Example: 15.7 cc’s x 3.5 = 55 ppb calcium carbonate
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6.2 Iodide Ion Analysis Procedure

Step 1. Use the routine horizontal core plug for iodide ion analysis. Re-dry the sample
if necessary.
Step 2. Allow the sample to cool and record dry weight.
Step 3. Disaggregate the sample to grains size with a Teflon, or rubber tipped, mortar
and pestle. Transfer disaggregated material to tared flask and weigh. Rinse mortar and
pestle with distilled water into flask and weigh again. Use 3 cm3 distilled water per
gram of rock.
Step 4. Extract with continuous shaking overnight in a wrist shaker.
Step 5. Analyze blank samples of distilled water for iodide using ion chromatography.
Step 6. Filter supernatant liquid (at least 10 cc) through 45 micron cellulose nitrate
cartridge filter.
Step 7. Provide the following data:
a. Dry weight for grain volume measurement including grain loss.
b. Crushed rock weight
c. Distilled water weight
d. Iodide concentration measured by ion chromatography
e. Dean Stark water volume
Step 8. Calculate concentration of iodide in Dean Stark water.
Clds = Concentration of Iodide in Dean Stark brine, ppm
Cle = Concentration of Iodide in extracted water, ppm
W s = Weight of salt in extracted brine, g IC analysis
W r g = Weight of grains in the core plug, g
W rc = Weight of crushed rock extracted, g
Wwds = Weight of water distilled in Dean Stark, g
Wwe = Weight of water used to extract rock, g
Step 9. Calculate filtrate saturation in core water from Dean Stark

Clcw = Concentration of Iodine in connate water, ppm

Clds = Concentration of Iodine in Dean Stark brine, ppm
Cl e = Concentration of extraction water, ppm
Clmf = Concentration of Iodine in mud filtrate, ppm
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dbds = Density of Dean Stark brine, g/cc

dbf = Density of Connate (formation) brine, g/cc
dw = Density of distilled water, g/cc
F = Fraction of filtrate in Dean Stark brine
fsds = Fraction of salt in Dean Stark brine
fsf= Fraction of salt in the connate (formation) brine
Sf = Filtrate saturation, %PV
Sdsw = Dean Stark water saturation, % PV
Step 10. Calculate corrected connate water: Scw = Sdsw - Sf
Note: If F exceeds 0.5 or Sf exceeds 10% pv then do not calculate connate water using
the above equation as it will be too low.
6.3 Bromonaphthalene Analysis Procedure
Scope: The purpose of this procedure is to provide accurate quantification of drilling
mud and cutting fluid invasion in core plugs. To accomplish this, a halogenated tracer
(1-bromonaphthalene) is added to the drilling fluid at a concentration of 100 ppm. Each
core sample is extracted with approximately 125 ml of reagent grade toluene. The
subsequent core extracts are analyzed by gas chromatography (GC) utilizing an electron
capture detector (ECD) and a Flame Ionization Detector (FID). The degree of core
invasion by the drilling mud is based on the concentration of tracer contained in the
toluene extract and the pore volume of the extracted core plug. In a similar fashion, the
cutting fluid (Isopar) invasion is based on the concentration of the Isopar in the toluene
extract.
Equipment models change with time, but this procedure should supply a good starting
point for the development of an acceptable analytical procedure.
Instrumentation—Hardware
Item 1. HP-5880A Gas Chromatograph—Level 4
Item 2. HP Model 7364 Autosampler
Item 3. HP Model 19312 Nickel 63 Electron Capture Detector
Item 4. PE/Nelson 25 m x.53 mm ID—0.5 m Film #N931-2689
Item 6. Valco 1/16" 304 stainless steel Tee
Item 7. HP Auto Sampler Vials and Caps
Item 8. 1 ml Glass Disposable Pipettes or Equivalent Eppendorf Pipettes
Reagents
Reagent 1. Bromonaphthalene; Eastman Part #2256
Reagent 2. Reagent Grade Toluene
Reagent 3. 1-Iododecane; Aldrich Part #23,825 -2
Reagent 4. 2 ppm Iododecane and 1.0% Squalane in Toluene
Reagent 5. Standards of 1-Bromonaphthalene (0.1 ppm to 10.0 ppm) in Toluene
and Crude Oil (20:1)
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Reagent 6. Field Crude Oil

Reagent 7. Squalane; Aldrich Part #23,431 – 1
GC—Conditions
Oven Profile
Initial Temp = 75° C
Initial Time = 2.00 min.
Program Rate = 20°/min
Final Temp = 300° C
Detector and Injector
Detector Temp = 325° C
Injector Temp = 300° C
Detector Attenuation = 28
Injection Volume = = 5.0 µl

Gas Flows
Column Flow = 9.5 cc/min.
Nitrogen Makeup = 100 cc/min.
Splitter Flow = 50 cc/min.
Septum Purge = 3.5 cc/min.
Analytical Procedure

1. Upon receipt each sample bottle is weighed to the nearest tenth of a gram and
recorded in a sample logbook. The samples will be refrigerated at all times when
not being processed.

2. a. A 0.5 ml aliquot of each sample is diluted 1:1 by volume with the internal
standard solution (i.e., 2 ppm Iododecane and 1.0% Squalane in Toluene).
b. In the case of the concentrated drilling fluid solutions it will be necessary to
pre dilute them0.4 g of sample to 10.00 g with reagent toluene. Actual weights
are recorded to the nearest milligram along with the respective dilution factor.

3. 5.0 µl of the sample/internal standard blend is injected into the GC splitter via
the auto sampler and data acquisition is initialized.

4. After the internal standard and tracer have eluted the three-port valve is actuated
and the oven temperature allowed to proceed to its maximum setting.

5. From the ECD, the concentration of the tracer is determined using the 1 ppm
iododecane peak as an internal standard along with the response factor relating
area counts to concentration. The internal standard is used to correct for
variations in sample size reaching the detector.
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6. From the FID, the concentration of the cutting fluid is determined using the
0.5% Squalane peak as an internal standard along with the response factor
relating area counts to concentration.

7. The measured tracer concentration is to be adjusted for any dilutions and then
reported as ppm tracer.

8. The measured cutting fluid's concentration is to be adjusted for any dilutions

and then reported as percent cutting fluid.

9. A three-point calibration curve of tracer in toluene and crude oil will be run
daily. Response factors will be calculated from the calibration curve and a
running log of the calculated response factors versus time will be maintained
daily.

References
1. Standard Procedure Ow Testing Drilling Fluids API R.P 1313 Dallas 1974
2. Drilling Fluid Tegineering Manual Magcobar Div. Dresser Industries Inc.,
Houston 1972
3. The ChevronTexaco and BP Drilling Fluid Manual