MEA CSL Stimulation Laboratory Procedures

SCHLUMBERGER MEA TECHNOLOGY HUBMEA STIMULATION CLIENT SUPPORT
MEA CLIENT SUPPORT LABORATORY

STIMULATION LABORATORY PROCEDURES
Prepared
by
Stimulation Section
MEA Client Support Laboratory
MEA Technology Hub
July 15, 2002

MASTER TABLE OF CONTENTS
SECTION 1 HYDRAULIC FRACTURING

HF-001 ClearFRAC Laboratory Preparation
HF-002 YF100HTD Laboratory Preparation
HF-003 YF800HT Laboratory Preparation
HF-004 YFGO”III” Laboratory Preparation
HF-005 YF100LG Laboratory Preparation
HF-006 YF100LGD Laboratory Preparation
HF-007 PrimeFRAC Laboratory Preparation
HF-008 SXE Laboratory Preparation
HF-009 Fann35 Linear Gel Viscosity Measurement
HF-010 Static Gel Break Test
HF-011 HTHP Gel Rheology Test (Fann50 Model Viscometer Operation)
HF-012 Fracturing Sand Sieve Analysis (API RP56/60)
HF-013 Proppant Sphericity and Roundness (API RP56/60)
HF-014 Silt Test  Turbidity Method (API RP56)
HF-015 Crush Resistance Test (API RP56)
HF-016 Crush Resistance Test (Testing RCP)
HF-017 Proppant Acid Solubility Test (API RP56)
SECTION 2 MATRIX ACIDIZING

MA-001 Hydrochloric Acid Laboratory Preparation
MA-002 Intensified Acid
MA-003 Clay Acid Laboratory Preparation
MA-004 Mud Acid Laboratory Preparation
MA-005 Oganic Mud Acid Preparation
MA-006 Oganic Clay Acid Preparation
MA-007 Alcoholic Acid Laboratory Preparation
MA-008 Gas Well Acid Laboratory Preparation
MA-009 Gas Well Mud Acid Laboratory Preparation
MA-010 Dowell Acid Dispersion (DAD)
MA-011 Demonstrating the Crosslinking of Leak-off Control Acid or Self-Diverting
Acid
MA-012 Breakdown Acid (BDA) Laboratory Preparation
MA-013 Mud Silt Remover Acid (MSR) Laboratory Preparation
MA-014 Non-Acid Reactive Solutions
MA-015 CLEAN SWEEP Fluids Laboratory Preparation
MA-016 Aqueous Acetic Acid Laboratory Preparation
MA-017 L036 Laboratory Preparation
MA-018 HCl Acid Strength Test
MA-019 Acid Solubility Test
MA-020 Determination of Total Iron
MA-021 Acid Corrosion Inhibitor Evaluation
MA-022 Scale Dissolution Capacity Tests (U104/U105/U106)
MA-023 Acid Response Test Procedure
2
SECTION 3 FOR MATION DAMAGE

FD-001 Immersion Test
FD-002 Mud Damage Laboratory Operation (can be adapted to MUDSOLV test)
FD-003 TEMCO ARCIII Tester Laboratory Operating
FD-004 Advanced Emulsion Tendency and Demulsification Test
FD-005 ClearFRAC Emulsion and Break Test
FD-006 Fluid Loss Testing (Microfracture simulation)
FD-007 Procedures for Compatibility of Formation Brine and Completion Brine
FD-008 Critical Velocity Determination for Fines Migration Study
FD-009 Determination of Critical Brine Concentration Determination for Swelling
Clays
FD-010 Dynamic Leak-off and Retain Permeability Testing
SECTION 4 CORE ANALYSIS

CA-001 Core Porosity Determination
CA-002 Gas Permeability Determination
CA-003 Rock Mechanics Test (dry core triaxial compression)
CA-004 SEM/EDAX Sample Preparation for Petrographic Core Analysis
CA-005 Bulk XRD Sample Preparation Procedures
CA-006 Total Clay Content Determination
SECTION 5 SAND CONTROL AND WATER CONTROL

SC-001 Semi-quantitative PSD Analysis by SEM Imaging
SC-002 Gravel and Screen Selection from PSD Information of Formation Sand
SC-003 Sand Settling Test
SC-004 K300 Sand Consolidation Testing
SC-005 SANDLOCK V Preparation Procedures
WC-001 Test Procedures for OrganoSEAL-R Working Time Determination (greater
than 100C)
WC-002 Test Procedures on Evaluation of OrganoSEAL-R Shut-off Effectiveness
WC-003 DGS Gel Working Time Determination
SECTION 6 ANALYTICAL METHOD

AM-001 Water Analysis
AM-002 Cloud Point Determination
AM-003 Methylene Blue Index Determination
AM-004 Vapor Pressure Measurement
AM-005 Determination of Asphaltenes and Paraffin Wax
AM-006 Scale/Solids Identification by XRD/Solubility/Water Analysis/EDAX
SECTION 7 LABORATORY SAFETY

LS-001 MEA Well Services Laboratory Audit
LS-002 MEA CSL Working Alone Procedures
LS-003 MEA CSL Typical Stimulation Chemicals Handling Guidelines
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SECTION 1 HYDRAULIC FRACTURING
HF-001 ClearFRAC Laboratory Preparation

Notes:
To convert gals per thousand gal of fluid to mililiters per 500 ml of fluid, divided by 2.
To convert pounds per thousand gal of fluid to grams per 500 ml, multiply by 0.06.
The following procedures are only for selected fracturing systems.
Equipment and Materials
Waring blender equipped with variable transformer
Blender jar
Graduated cylinder and syringes
Timer
PH meter
Thermometer
Fann35
Additives in ClearFRAC system
Code Function Example Concentration Amount in 500ml
M117 Potasium chloride 333 lb/Mgal 20 g
J508 Gelling agent 4.0 gal/Mgal 2.0 ml
J463 (T>150F) HT activator 5 lb/Mgal 0.3 g
Preparation Procedures
• Pour 500ml of water into the blender jar and stir.

• Add 20 grams of KCl and dissolve.
• Or add 0.3 gram of J463 and dissolve it if the fluid temperature greater than
150oF.
• Create a vortex to the tip of the stirrer. Slowly add J508 into the brine. The
concentration will depend on the desired viscosity.
• Stir the mixture until the vortex is closed.
• Place the mixture into water bath at 70-80C to get the foams out and the fluid
becomes clear.
• Check the fluid temperature and pH.
• Check the fluid viscosity to see if it is in the specified range (See Fann 35 test
procedures).
4
HF-002 YF100HTD Laboratory Preparation

Blender jar
Timer
PH meter
Thermometer
Fann35
Example---Additives in a typical YF140HTD system
Code Function Concentration Amount for 500ml
M275 Microbiocide 0.45 lb/Mgal 0.027 g
J353 HT gel stabilizer 10 lb/Mgal 0.6 g
F75N surfactant 1 gal/Mgal 0.5 ml
J424 Gelling agent 40lb/Mgal 2.4 g
L10 crosslinker 7.5 lb/Mgal 0.45 g
M2 activator 15 lb/Mgal 0.9 g
J450 stabilizer 1 gal/Mgal 0.5 ml
J480 Crosslink delay agent To be determined To be determined
J490 Encap-breaker To be determined To be determined
Linear Gel Preparation
• Pour 490ml water into the mixing cup. Stir with low speed.
• Add 10 grams of KCl and 0.027g of M275 into the mixing cup.
• Add 2.4g of J424 slowly into the cup and control the stir rate to allow the polymer
dispersion.
• Increase the stir rate after polymer dispersion to get faster hydration.
• Hydrate the gel for 30-60 minutes.
• Check the fluid temperature and pH (should be 6-8).
• Check the fluid viscosity to see if it is in the specified range against FMM spec.
(See Fann 35 test procedures).
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• During the gel hydration, weigh 0.6g of J353, dissolve it using small amount of
water.
Crosslinker Preparation
• Add 3.7ml of water into a glass bottle. Start stirring using magnetic stirrer.
• Weigh 0.9g of M2 and add slowly into the bottle while stirring.
• Measure 0.45g of L10, add it into the bottle while stirring.
• Add the required amount of J480 slowly for dissolving. Place 0.5ml of J450 into
the bottle after J480 dissolving.
• Age the crosslinker solution for 60min.
Gel Crosslinking
• Adjust the stirring speed to create a Votex to the tip of the stirrer.
• Add J353 solution and 0.5ml of F75N into the mixing cup to mix one more minute.
• Add the prepared crosslinker into the linear gel while start timing.
• Record the time to reach the vortex closure. (Votex Closure Time)
• Check the time until hang-lip happens. (Hang-Lip Time)
• Check the pH of the X-linked gel.
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HF-003 YF800HT Laboratory Preparation

Blender jar
PH meter
Thermometer
Fann35
Additives in a typical YF845HT system

Code Function Concentration Amount for 500ml
M275 Microbiocide 0.45 lb/Mgal 0.027 g
F75N surfactant 1 gal/Mgal 0.5 ml
J916 Gelling agent 10.1 gal/Mgal 5.05ml
L401 buffer Adjust to pH 6.5-7.0
J353 HT gel stabilizer 10 lb/Mgal 0.6 g
J464 activator 10 lb/Mgal 0.6 g
M2 (2%) activator 10 gal/Mgal 5 ml
J450 stabilizer 1 gal/Mgal 0.5 ml
J515 crosslinker 0.7 gal/Mgal 0.35 ml

• Pour 490ml water into the mixing cup. Stir with low speed.
• Add 10 grams of KCl and 0.027g of M275 into the mixing cup.
• Measure 5.05ml of polymer slurry and add slowly into the cup and control the stir
rate to allow the polymer dispersion. Check the pH of the fluid while adding L401
until the fluid pH of 7.0, record the pH.
• Increase the stir rate to get faster hydration and hydrate for 30 minutes.
procedures), record linear viscosity against FMM spec, pH (6.9-7.1) and
temperature.
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• During the gel hydration, weigh 0.6g of J353, 0.6g of J464, dissolve each of them
using around 2 ml of water.
• After gel hydration (meet the spec.), Add the above J353 solution, F75N (0.5ml)
into the linear gel in the order. Stir it for about two minutes and check pH again.
Gel Crosslinking(recommend using microwave)

• Heat the water bath to around 90oC or using a microwave oven for homogeneous
heatup.
• Add J464 solution, M2 (2%), 0.5ml of J450 and 0.35ml of J515 into the above
linear gel. Check pH after addition of each component.
• Continue to mix the fluid at a vortex (to the tip of stirrer) for 30sec more after
adding J515 and check fluid pH.
• Split the as-prepared mixture into two parts. Using 300ml to do the X-linking test
and another part to do the Fann50 test.
• Start Fann50 test ASAP after above fluid mixing, Try best to reduce the time
duration between end of fluid mixing and Fann50 starting (3-5 minutes).
• Place the beaker containing 300ml of as-prepared gel into the water bath or
microwave.
• Hand-shaking the fluid to avoid temperature gradient from wall of the beaker to
center of the fluid. Check the X-link everything 15-30 seconds (adjust the time
while using microwave) while testing the fluid temperature by thermometer.
• Write down the fluid temperature while there is a noticeable resistance in the way
that thermometer moves into/out of the fluid.
8
HF-004 YFGO”III” Laboratory Preparation
Introduction
YF’GO”III* is a gelled, oil-base fluid originally designed as a fracturing fluid for the
treatment of water sensitive formations. Diesel, kerosene, condensate and a wide
variety of crude oils can be used to prepare YG’GO”III.
Safety
Oil-base fluids can irritate skin, wear protective gloves and safety glasses. Read the
Dowell Material Safety Data Sheet of each additive before using.
Disposable syringes
Glass or plastic beakers
Magnetic stirrer
Balance
Waring blender
FANN 35 viscometer
Graduated measuring cylinders
Water bath
J452 Oil Gelling agent
J601 Crosslinker
J602L pH Control Agent
M003 Breaker
Mixing Procedures
• Mixing of Activator Solution

The activator solution is prepared by mixing J602L and J601 at a ratio of 1:5 by
volume (if J602 solid is to be used, mix 1.44g of J602 in 10mL of deionised water and
mix until dissolved, this is then equivalent to J602L). Place a small glass beaker on
the magnetic stirrer and add the following additives:
J602L 2mL
J601 10mL
Allow this solution to mix for at least 30 minutes.
• Batch Mixing of YF”GO”III Fluid
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YFGOIII is prepared by simultaneously adding J452 Gelling Agent and activator

solution to the base fluid (normally diesel containing <0.5% water since the system is
water sensitive).
• Place 1L of diesel in a Waring Blender and start mixing at 2000rpm. Create a
vortex down to the blades.
• Simultaneously add the desired quantity of J452 and activator solution to the
edgw of the vortex. The quantities required to produce a 6, 7 or 8 gal gel per
1000 gal of diesel are listed in the following (Equivalent to 6, 7 or 8mL per
1000mL)
J452 (mL/1000mL diesel) Activator (mL/1000mL diesel)
6 3
7 3.5
8 4
• Mix at 10,000 rpm for 10 minutes.

• Transfer gel to a Fann 35 cup and measure viscosity developed at 170 sec-1.
The following lists the desired viscosity for 6, 7 or 8 gal gels.
J452 (mL/1000mL) Viscosity (cP @170sec-1 @ 21°C)
6 100 - 120
7 120 - 140
8 140 - 170
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SCHLUMBERGER MEA TECHNOLOGY HUBSTIMULATION CLIENT SUPPORT
HF-005 YF100LG Laboratory Preparation
Introduction
The Widefrac 100 (YF100LG) fracturing fluids are water-based systems composed of
a refined guar gelling agent crosslinked by a borate crosslinker. They are prepared
from the Waterfrac 100 fluids. YF100LG fluids are designed to crosslink quickly. The
vortex closure of these fluids is 5 to 10 seconds which allows uniform mixing of all
components before becoming viscous. The crosslink is fairly mature in another 10 to
20 seconds.
Safety
Normal safety procedures should be observed. the minimum eye protection is safety
glasses. Flush eyes with water immediately if contacted with materials used in test.
Wash affected skin with water.
Waring blender
Blender cup
Graduated cylinders
Disposable syringes
pH meter or paper
Water gelling agent J424 or PSG Polymer Slurry J877
Mixing Procedures
• Crosslinker
Crosslinker L010 at 1.2 to 2.2 lb L010/1000gals WF100 fluid (0.144 to 0.264g
L010/Litre) depending on temperature.
For addition of small quantities a stock solution of L010 can be prepared by adding
2.3965 g of L010 to 100 mL of distilled water.
1mL L010 stock solution per 200 mL of WF100 = 1 lb L010/1000 gals WF100
• Crosslinker Activator
The pH stabilizer (activator solution) for fracturing temperatures less than 175°F
(79°C) contains J494 at 12lb/1000gal (of YF fluid) and M3 at 5lb/1000 gal of (YF
fluid). This is called a 12-5 solution. The preferred way to add the J494 and M3 to
the fluid is to prepare a 14 to 20% (wt/wt) aqueous solution and meter it in at the
blender.
To prepare a 16% (wt/wt) 12-5 solution:
--- Place 19mL of deionised water in a small glass beaker on a magnetic stirrer.
--- Slowly add 2.55g of J494 to the vortex.
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--- Slowly add 1.06g of M3 to the vortex.

--- Continue mixing for 15-20 minutes until the solids have dissolved.
The specific gravity of a 16% (wt/wt) solution at 75°F is 1.131g/cm3. An addition rate
of 11.3 mL/1000mL of linear gel is equivalent to 12lb J494 and 5lb M3 per 1000gal of
fluid.
• Breaker Solution
A solution of J218 can prepared by adding 2.3965 g of J218 to 100 mL of distilled
water.
1mL J218 stock solution per 200 mL of WF100 = 1 lb J218/1000 gals WF100
• Prepare 500 mL of WF100 base gel.
• Add L010 to the base gel and mix at low speed for one minute, ensuring air is not
trapped.
• If J218 breaker is required add to the vortex and mix for one minute.
• Set the mixer speed to 1900-2000rpm and add 5.65mL of the J494:M3 activator
solution to the vortex. A vortex closure of 10-15 seconds should be observed.
After 30 seconds, stop the mixer and transfer the fluid to a beaker. The fluid
should be fully crosslinked.
• Check the pH of the crosslinked fluid. It should be 9.6 to 9.9 at ambient
temperature.
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HF-006 YF100LGD Laboratory Preparation
Introduction
The Widefrac 100 (YF100LGD) fracturing fluids are water-based systems composed
of a refined guar gelling agent crosslinked by a borate crosslinker. They are prepared
from the Waterfrac 100 fluids.
Safety
Normal safety procedures should be observed. the minimum eye protection is safety
glasses. Flush eyes with water immediately if contacted with materials used in test.
Wash affected skin with water.
Waring blender
Blender cup
Graduated cylinders
Disposable syringes
pH meter or paper
Water gelling agent J424 or PSG Polymer Slurry J877
Mixing Procedures
• Crosslinker
The crosslinker solution consists of:
Water (4.5 to 7 gal/1000gal).
L010 at 5.5 to 9.0 lb L010/1000gals WF100 fluid (0.659 to 1.078g L010/Litre)
depending on temperature.
Activator M2 (10 to 20lb/1000gal) or U28.
Stabilizer J450, typically 1 gal/1000gal (if required).
For example:
Fresh water 6gal 6mL
L10 7lb 0.84g
M2 16.5lb 1.98g
J450 1gal 1mL
The above solution, before the J450 is added, has a specific gravity of 1.304 at 24°C
and therefore will have an addition rate of 7.8gal/1000mL (or 7.6mL/1000mL).
Calculated as follows:
Crosslinker rate = weight of crosslinker solution / 1000 gal
8.34 x S.G.
= (6 x 8.34) + 7 + 16.5/(1.304 x 8.34) = 6.8 gal / 1000 gal
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with 1gal/1000 J450 = 7.8 gal/1000gal (or 1.56mL/200mL)

• Crosslinker Delay Solution
• The delay agent J511 concentration depends on the polymer concentration, mix-
water temperature and desired crosslink time. The minimum J511 concentration
required to prevent syneresis (over crosslinking) at room temperature for
approximately 12 hours is 10lb/1000gal. J511 is readily soluble in water. The
addition of NaOH at about 1lb/1000gal prevents the deterioration of the J511
solution by bacteria (~pH 10). Aqueous solutions having 30-70% J511 present
can be employed. A 30% solution contains 2.79lb J511/gal and can be prepared
in the laboratory as follows:-
To 70mL of water, add 0.02g of M2 and allow to mix.
Add 30g of J511 and continue mixing until all solids have dissolved.
The following table can be used as a guideline for adding various quantities of
J511:
Desired concentration Equivalent to gal of 30% Equivalent to mL of 30%

J511 (lb/1000gal) J511 / 1000gal of WF100 J511 / 200mL of WF100
10 3.6 0.72
15 5.4 1.08
20 7.2 1.44
25 8.9 1.78
30 10.7 2.14
• Breaker Solution
A breaker solution can prepared by adding 2.3965 g of J218 or J481 to 100mL of
distilled water.
1mL J218 or J481 stock solution per 200 mL of WF100= 1 lb J218 or J481/1000
gals WF100
• Crosslink Delay Procedure
In order to determine the crosslink delay times with various concentrations of
J511 present, the following procedure should be followed:-
--- Place 200mL of the WF100 fluid into a Waring Blender jar, record fluid
temperature.
--- Start mixing at 2000rpm, this should produce a vortex.
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--- Inject the delay agent and blend for 2 minutes.

--- Inject the crosslinker solution and start the stopwatch simultaneously.
--- Vortex closure is when the crosslinked gel covers the blade nut 50% of the
time. Record the time.
--- When vortex closure is achieved, stop blender and pour gel into 250mL
beaker.
--- Pour fluid from one 250mL cup to another until 80% crosslink is achieved.
(80% crosslink = when gel is poured, the floppy gel is easily retractable into the
cup and shows no adhesion to the wall of the cup). Also notice if the crosslinked
gel can be fractured during the floppy test. Record the time to 80% crosslinking.
• Continue pouring the crosslinked gel from cup to cup every 15 seconds until
100% crosslinking is achieved (100% crosslink = when crosslink gel is poured
from cup to cup and fluid comes out as one solid mass with minimal elongation).
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HF-007 PrimeFRAC Laboratory Preparation

Blender jar
PH meter
Thermometer
Fann35
Microwave
Titrator
0.1N HCl
Methyl orange indicator
Phenolphthalein indicator
Orion Model 130A conductivity Meter
Fluid additives and RCP

• Pour amount of water (pH 6-8, adjust by HCl or NaOH if not in the range) into the
mixing cup. Stir with low speed. Add D047 if needed.
• Add required KCl, M275, F103 and J353 in sequence into the mixing cup.
• Measure polymer slurry and add slowly into the cup and control the stir rate to
allow the polymer dispersion. Check the pH of the fluid while adding J488 until
the fluid pH of less than 7.0, record the pH and the amount of J488 needed for
pH adjustment.
• Increase the stir rate to get faster hydration and hydrate for about 10-15 minutes.
procedures), record linear viscosity against FMM spec (170sec-1 and 511sec-1),
pH and temperature.
• Continue mixing for another 5 minutes until the viscosity meet the specification.
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Gel Crosslinking and Delaying

• Fill blender with 250ml linear gel as-mixed, shear at low speed.
• Add J464 solution, J494 solution and J513 into the above linear gel. Check pH
after addition of each component.
• Continue to mix the fluid at a vortex (to the tip of stirrer) for 20-30 sec after adding
J513 and check fluid pH.
• Split the as-prepared mixture into two parts. Using 100ml to do the X-linking test
and another part to do the Fann50 test.
• Start Fann50 test ASAP after above fluid mixing, Try best to reduce the time
duration between end of fluid mixing and Fann50 starting (3-5 minutes).
• Place the beaker containing 150ml of as-prepared gel into the microwave.
• Check the X-link everything 5-10 seconds while testing the fluid temperature by
thermometer.
• Write down the fluid temperature (supposed to be less than 120F for better fluid
stability) while there is a noticeable resistance in the way that thermometer
moves into/out of the fluid (100% X-linked).
RCP/PrimeFRAC Compatibility
• Fill blender cup with 250ml linear gel as-mixed. (refer to linear gel preparation)
• Add required amount of J464L and J494L, mix at low speed.
• Add 1PPA RCP into the blender, increase mixing speed for deep votex to shear
for 2-3 minutes.
• Add J513 into the blender in the last few second during above shearing.
• Static settling for about 2 minutes.
• Centrifuge above mixture at 1500rpm for 3-5 minutes.
• Decant the clear part of the mixture. Check pH to make sure in the range of 9.2-
9.5, otherwise adjust with J494L to meet pH requirement and record the amount
added.
• Take about 150ml above gel into the beaker and place it into the microwave for
X-link temperature determination as above. (refer to X-link and Delaying Test)
• Change J464L concentration and repeat above steps if X-link temperature does
not meet the specification (less than 120F). Otherwise go to nest step.
• Take amount of fluid (about 35mls), add required breaker to run Fann50 tests.
• Increase proppant adding as FracCADE design to check all loadings (for
example, 2PPA, 4PPA, 6PPA, 8PPA, 10PPA, 12PPA). Repeat above testing
17
procedures to get a detailed relationship between RCP loading and gel X-link/gel
stability.
18
J464L/J494L/J513 QA/QC
J464L (J464 at 0.50lb/gal)
• Dilute 1ml of J464L sample to approximately 50ml of DI water.
• Add 4 drops of methyl orange indicator to shake to homogeneous.
• Titrate with 0.1N HCl standard solution until from orange to pink (endpoint, about
6.7ml).
• Calculate the concentration
ml of 0.100N HCl × 0.0742 = lb of J464/gal
• Acceptable if within ±10% of specification.
• Adjust field J464L rate based on above results.
J494L (J494 at 1lb/gal)
• Dilute 1ml of J494L sample to approximately 50ml of DI water.
• Add 4 drops of Phenolphthalein indicator to shake to homogeneous (turns pink).
• Titrate with 0.1N HCl standard solution until from pink to colorless (endpoint,
about 5.6ml).
• Calculate the concentration
ml of 0.100N HCl × 0.1786 = lb of J494/gal
• Acceptable if within ±10% of specification.
• Adjust field J494L rate based on above results.
J513 solution
• Prepare standard J513 solutions (15%, 25%, 35% and 50%) using 100ml
volumetric with location water being used to dilute J513.
• Measure the conductivity using conductivity meter on the standard J513 solutions
as-prepared above.
• Prepare a standard curve of conductivity vs. temperature for various J513
concentrations.
• Measure the conductivity of the field prepared J513 solution.
• Determine the volume% of J513 for the field prepared J513 solution from the
standard curve. (additional check on SG should be completed to verify the field
sample)
• Calculate the concentration of J513 in the field sample. Acceptable if within ±10%
of specification.
Vol% J513 determined in step above = gal J513/gallon of the field sample
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Conductivity and Specific Gravity for J513 Standard Solutions

J513 Conductivity (milli-siemens) Specific
solution 75F 100F 120F Gravity
(vol%)
15 29.7 37.9 45.9 1.01
25 41.3 53.1 65.1 1.03
35 49.2 64.6 77.5 1.05
50 55.8 --- --- 1.08
Typical J513 Standard Curve
80
70
Conductivity (milli-siemens)
15%
25%
60 35%
50
40
30
20
50 60 70 80 90 100 110 120 130
Temperature (F)
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HF-008 SXE Laboratory Preparation

Introduction
SXE (Super X Emulsion) from Schlumberger is an oil-external emulsion formed with
70:30 HCl to oil ratio, stabilized with an emulsifier. The acid concentration can be
ranged from 7.5% to 28%.. As high as 13-fold retardation acid reaction can be
achieved for 28% HCl SXE. Even high retardation is achieved for lower acid
concentrations. Laboratory preparation of SXE emulsified acid is described in this
procedure.
Safety
Goggles, rubber gloves and a protective covering must be worn when mixing acids.
Always work under a fume hood when preparing acids.
ALWAYS ADD CONCENTRATED ACID TO WATER.
350ml beakers
Syringe and 15ml glass tubes
magnetic stirrer
PMC hot-plate stirrer with speed adjustment
Fann35 with Hestolloy bob/sleeve and fluid cup
Kerosene or diesel
HCl (7.5% to 28%)
A166 (inhibitor)
U080 emulsifying agent
Glass rod
2% KCl
Mixing Procedures
• Add 140ml HCl into glass beaker, mix with magnetic stirrer to get a votex to the
stirrer bar. Add corrosion inhibitor as required to mix homogeneously.
• Place another beaker on the mixing plate and place 60ml kerosene and U080
into the beaker to mix thoroughly with votex tip to the bottom of the beaker.
• Use syringe to drop the acid mixture (acid+inhibitor) into the oil/U80 mixture while
stirring with the tip of the votex to the beaker bottom.
• Increase the mixing speed as high as possible after adding all acid mixture into
the oil mixture for about 15-20 minutes. A stable emulsion system is supposed to
be prepared.
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• Sample the mulsion into the 15ml glass tube to observe for 10 minutes. No
separation will be evident if the emulsion is an oil-external stable emulsion.
• Another way to check the oil-external property is tick a drop of emulsion using the
glass rod and drop it into a 2% KCl solution in the 15ml glass tube, the drop will
remain and slowly settle down to the tube bottom if an oil-external emulsion
forms, otherwise it will disperse quickly into the solution.
• Change the oil source (some commercial diesel is contaminated and not suitable
for SXE preparation) if getting a hard time to form a stable oil-external emulsion.
• Check Fann35 rheology using the hestolloy bob/sleeve combinations if a stable
oil-external emulsion forms.
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HF-009 Fann35 Linear Gel Viscosity Measurement

Introduction
The most commonly used viscometer in testing fracturing fluids for their low
temperature rheology is Fann35 viscometer. Generally six rpms are available, which
are 3, 6, 100, 200, 300, 600rpm. The calculation of the viscosity based on the
viscometer reading is stated in the Calculation section.
Fann35 viscometer with appropriate parameters (speed factor, R-B factor and spring
factor)
Rotor and bob
Fann35 sample cup
Fracturing fluid
Thermometer
Test Procedures
• Power on the machine (check the power volts required, 110v/220v A.C.?)
• Install rotor and bob.
• Fill the sample cup to the mark with fracturing fluid.
• Place the cup containing sample on the stage (three pins on the bottom of the
cup sit in three holes on the stage)
• Raise the stage until sample is at the mark on the rotor.
• Set Fann35 to the desired shear rate. Shift gears only when the instrument is
running.
• Let dial come to a steady reading and record.
• Record the fluid temperature using thermometer.
• Turn off the machine and clean all parts of the instrument.
• Calculate the viscosity.
Calculation
The fluid viscosity can be determined by the following equation

η = S × φ × f × C, Where
η, fluid viscosity, cp
S, Speed factor,
f, spring factor
C, rotor-bob factor
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φ, dial reading
The above factors can be found in the following table.
Torsion Spring Rotor Rotor-Bob
Spring No. f rpm S Combinatio C
n
F0.2 0.2 0.9 333.3 R1-B1 1.000

F0.5 0.5 1.8 166.6 R1-B2 8.915
F1 1 3 100 R1-B3 25.392
F2 2 6 50 R1-B4 50.787
F3 3 30 10 R2-B1 0.315
F4 4 60 5 R2-B2 8.229
F5 5 90 3.33 R2-B3 24.707
F10 10 100 3 R2-B4 49.412
180 1.667 R3-B1 4.517
200 1.5 R3-B2 12.431
300 1.0 R3-B3 28.909
600 0.5 R3-B4 57.815
Chan35 - Linear Gel Viscosity Test
24
HF-010 Static Gel Break Test
Introduction
This is important for the field operation without HTHP gel break test equipment. A gel
is usually considered broken enough to flow back when it has been degraded to a
viscosity of 20cp at required temperature. (as close as possible to BHT for the initial
PPA stage, decrease temperature for the following stage of PPA by FracCADE
simulation)
1000ml jar with cap

200ml high temperature bottles
HTHP fluid loss cell and heating jacket
Fann35 with proper accessories
Water bath with temperature control
Thermometer
Stop watch
Gel and breaker being tested
Test Procedures (for temperature less than 100C)
• Prepare the base gel as described in different fluid preparation procedures.

• Place amount of breaker solution (dissolve J218 or J481into small amount of
water, use equivalent amount of J218 and J481 if J475 and J490 Encap-breaker
are used, refer to FMM for Encap breaker release rate) into the linear gel before
adding the cross-linker solution.
• X-link the gel as described procedures in according fluid preparation procedures.
• Preheat the water bath to the required temperature.
• Pour 500ml of gel into the loosed covered jar.
• Place the jar containing gel in the water bath that will bring the sample to the
required temperature. Stir it slowly while heating to accelerate the process.
• Start timing while temperature reach the BHT.
• Tight the jar cap.
• Shake the jar vigorously every 30 minutes and visually observe the viscosity.
• Install Fann35 rotor, bob and sample cup.
• Take appropriate amount of gel from the jar and place it into the heated sample
cup.
25
• Start testing the fluid viscosity at 170sec-1 as quick as possible when fluid
temperature is at required temperature.
• Continue the above process until fluid viscosity reaches 20cp. Write the time,
which is the static gel break time.
Test Procedures (for temperature greater than 100C, qualitative method)

• Prepare the base gel as described in different fluid preparation procedures.
• Place amount of breaker solution (dissolve J218 or J481into small amount of
water, use equivalent amount of J218 and J481 if J475 and J490 Encap-breaker
are used, refer to FMM for Encap breaker release rate) into the linear gel before
adding the cross-linker solution.
• X-link the gel as described procedures in according fluid preparation procedures.
• Preheat the heating jacket to the required BHST.
• Place the X-linked gel into the HT bottle with finger-tight cap and put them into
the HTHP fluid loss cell containing proper amount of oil whose level is right below
the bottle cap connection to avoid oil getting into the bottle and contaminate the
fluid. Keep the whole cell assembly straight during above operation.
• Place the HTHP cell assembly with bottle/oil heating medium into the heating
jacket, again, keep all operating straight.
• Start timing while HTHP cell temperature reach the BHT.
• Visually observe the viscosity of the fluid by cooling down the cell and taking out
the bottle after expected breaking time.
• Judge if is broken by lab experience.
26
HF-011 HTHP Gel Rheology Test (Fann50 Model Viscometer Operation)
Introduction
The HTHP fluid rheology tester in our lab is NI HTHP Rheometer with the capability
of up to 260oC and 1000psi fluid test. The day-to-day use of this instrument for
stimulation is performing x-linked gel breaking test when BHT is required above
100oC.
The machine should be calibrated at the regular base (daily calibration should be
performed if high volume of test is run.). See instrument manual for calibration
procedure.
The temperature deviation should be less than 5oF, rerun the calibration if not.
Parameters A and B from calibration report should be greater than 0.999 and
viscosity deviation should be less than 3.0%, either rerun the calibration or rebuild
the head assembly if not in the above specification range. Refer to NI Rheometer
Manual for Rebuilding Head Assembly.
NI HTHP Rheometer with appropriate parameters (speed factor, R-B factor and
spring factor)
Rotor and Bob5 or Bob-5X
Fracturing fluid being tested
Test Procedures
• Power on the machine and computer until NORDDAQ program manager.

• Supply water and N2 (450psi generally, 800psi for Encap-breaker) after the
machine is calibrated properly (see Rheometer manual for proper calibration
procedures).
• Prepare the X-linked fracturing fluid as described in specific fracturing fluid lab
preparation procedures.
• Activate NORDDAQ program, click on “operating menu” followed by “heat bath”.
Type in the required temperature and start preheat the oil bath.
• Place about 26mls (for Bob5) of X-linked gel inside the rotor cup followed by the
required amount of Encap-breaker.
• Place another around 26mls of X-linked gel into the rotor cup.
• Screw the bob (counter-clockwise) to the shaft until its finger-tight.
• Slowly screw the rotor containing the sample to expansion fitting to a little tight.
• Take off the cover of the oil bath, close the glass door.
27
• Go to “operating menu” “custom” (or “API”) we prefer all tests by “API” setting
except for client specific request. API ramp should be 118rpm (100sec-1),
88.5rpm (75sec-1), 59rpm (50sec-1), 29.5rpm (25sec-1), 59rpm (50sec-1), 88.5rpm
(75sec-1), 118rpm (100sec-1).
• Choose the correct “bob” (bob5), “interval stir rate” (118rpm) and “final
temperature setpoint”.
• Click “Initial test” in the operating menu followed by “yes” and “OK” to go to
“ASCII FILE” and “report printout”. Choose the options we need.
• Follow the screen until “perform test” showing up and click it.
• The instrument will automatically be running until the program has been finished
and print out the results by itself.
• If operator wants to stop the machine during testing, go to “operating menu” and
click “shut down”.
• Click on “file” on the top of screen and find “reprint report”. Click it and print out
the report manually.
• Allow the machine cool down to below 100oF. Release pressure and close the
water line.
• Dissemble rotor cup and bob gently and clean them up.
• Turn on the Nitrogen to 10-20psi to get all excess water or gel residue out of the
expansion fitting.
• Spray some WD40 on the shaft to lubricate the bearing. Using paper towel to
wipe off the moisture and gel on the shaft very gently (do not press against the
shaft. Clean everything leftover and cover the oil bath.
• Turn off the machine and release the pressure in the main N2 line.
Calculation
The floowing equations are used in the instrument for calculation

γ = k3 × RPM
τ = T × 980.665 / factor
ν = 47880 × K’ / γ1-n’
k3 = π / [15 × (Rr2 – Rb2)]
factor = surface area × bob radius
28
NI Rheometer – HTHP Fracturing Fluid Rheology Test
29
HF-012 Fracturing Sand Sieve Analysis (API RP56/60)
Introduction
Calibrated ASTM sieves are used to test the particle size distribution of the fracturing
sand/proppant. A minimum of 90wt% of the tested sample should fall within the
designating sieve sizes. Not over 0.1 wt% of the total tested sand sample should be
larger than the first sieve size and not over 1 wt% should be smaller than the last
sieve size.
Refer to API RP56 for recommended sieves used in testing designated sand sizes.
Refer to API RP60 for recommended sieves used in testing designated HSP sizes.
Sieve set of appropriate sizes for product to be tested (Refer to ASTME E 11-95).
Testing sieve shaker that provides simultaneaous rotating and tapping action and
accepts the sieves designated. The shaker shall be calibrated to the following
specifications: revolutions/min = 290+/-, taps per min 156+/-, height of tapper =
33.4mm (1,032 in) and timer accurate to 5 seconds +/-.
ASTM standard sieves
Endecotts test sieve shaker
Balance
Split sand/proppant sample
Test Procedures
• Refer to API RP56/60 to find the recommended sieves used in testing designated
sand sizes.
• Obtain a split sample of approximately 100 grams and establish an accurate
weight (W T) to within 0.1 gram.
• Weigh each sieve accurately. Be assure that all sieves are completely cleaned by
the manufacturer recommended brush.
• Pour the sample onto the top sieve and place the recommended sieve set plus
the pan in the test sieve shaker. Cover the sieves and tight the sieve set.
• Power on the sieve shaker for 10 minutes.
• Remove each sieve and weigh it accurately, be reminded of brushing off the
particles from bottom-side of each sieve to the next size.
• Calculate the percentage by weight of the total sand sample retained on each
sieve and in the pan.
• The cumulated weight should be within 0.5% of the sample weight used in the
test, if not, the sieve analysis must be repeated using a different sample.
30
Calculation
weight of the retained sand (W R) = sieve weight after shaking – sieve weight before
shaking
wt% of the total sand sample retained on each sieve = W R / W T × 100
Recognized Fracturing Sand Sizes
Sieve opening 3350/ 2360/ 1700/ 1180/ 850/ 600/ 425/ 212/
sizes 1700 1180 850 600 425 300 212 106
Frac sand size 6/12 8/16 12/20 16/30 20/40 30/50 40/70 70/140
designations
4 6 8 12 16 20 30 50
6 8 12 16 20 30 40 70
USA sieves 8 12 16 20 30 40 50 100
recommended 10 14 18 25 35 45 60 120
12 16 20 30 40 50 70 140
16 20 30 40 50 70 100 200
pan pan pan pan pan pan pan pan
Recognized High Strength Proppant Sizes
Sieve opening sizes 1700/850 1180/850 850/425 425/212

Opening size, inch 0.0661/0.0331 0.0469/0.0331 0.0331/0.016 0.0165/0.008
5 3
Frac sand size 12/20 16/20 20/40 40/70
designations
8 12 16 30
12 16 20 40
USA sieves 16 18 30 50
recommended 18 20 35 60
20 25 40 70
30 30 50 100
pan pan pan pan
ASTM Standard Sieves and Endecotts Sieve Shaker
31
HF-013 Proppant Sphericity and Roundness (API RP56/60)
Introduction
Particle sphericity is a measurement of how closely a sand particle or grain

approaches the shape of a sphere. Grain roundness is a measure of the relative
sharpness of grain corners, or of grain curvature.
See API RP56 /60 for the test method. (Krumbein and Sloss visual estimation
method)
Minimum 0.6 of both sphericity and roundness is required by API.
Equipemnt and Materials
Optical microscope, Heerbrugg, Model Wild M3/or SEM, phillips, Model XL30
Sample sticker/platform
Proppant sample
Test Procedures
• Stick 20 or more grains of proppant on the glass plate (platform for ESEM).
• Switch on the optical microscope. (refer to SEM analysis for ESEM start up
procedures)
• Adjust the magnification to suitable setting until a clear picture of proppant
particles show up.
• Compare the shape of the particles visually with the standard chart (see API
RP56, pp7) and determine the sphericity and roundness of each particle.
• Take the average of the above reading as the sphericity and roundness of the
proppant sample.
32
Optical Microscope for Particle Sphericity and Roundness
33
HF-014 Silt Test  Turbidity Method (API RP56)

Introduction
Turbidity in water is the result of suspended clay, silt, or finely divided inorganic
matter being present.
HACH spectrometer is employed to measure the optical property of the above
suspension, giving us a turbidity of the tested proppant sample.
The turbidity of the tested proppant sample should be 250 FTU or less.
HACH DR2000 and sample vials
About 6-ounce plastic capped wide-mouth bottle
Syringe/pippet
DI water and proppant sample
Test Procedures
• Measure 20ml of dry proppant sample and mix with 100ml of DI water in a 6-
ounce wide-mouth bottle, allow to stand for 30 minutes.
• Shake vigorously by hand for 45-60 shakes in 30 seconds, allow to stand for 5
minutes.
• Switch on the HACH DR2000.
• Dial the program number of 750 and set the wavelength to 450nm.
• Zero the FTU by using DI water in the test vial.
• Using a syringe or pippet, extract 25mls of water-silt suspension from near the
center of the water volume.
• Place the water-silt suspension in the test vial.
• Determine the sample turbidity in FTU.
HACH2000 Spectrophotometer for Turbidity Test (also for water analysis)
34
HF-015 Crush Resistance Test (API RP56)

Introduction
Crush resistance is a measure of fracturing sand strength under the designated
stress.
A given amount of sand particles within the designated sieve range is required for the
test.
Samples of sand subjected to the stress specified in API RP56, Table 3 should not
produce more than the suggested maximum fines (wt%) as prescribed in the table for
the sand size being tested.
Pan and two U.S.A sieves (as defined in ASTM E 11-81) of the mesh size opening
for the specified sand size range, for example, No.12 and No.20 for 12/20 sand.
Endecotts Test Sieve Shaker
Balance
Perrier Model 14570 hydraulic press
2-inch test cell with piston
Split sand sample
Test Procedures
• Stack the designated sieves and pour sufficient sample on the top sieve.
• Discard the particles on the top sieve and passing through the bottom sieve.
• Weigh 40g of as-sieved sample and place it into the test cell, constantly moving
the source of the sample to keep the surface inside the cell as level as possible.
• Insert the piston into the cell without applying any force. Rotating the piston 180o.
• Without shaking or jarring the cell. Place the cell containing the piston and
sample in the press.
• Apply the required load as defined in API RP56, TABLE 3 for the tested sample.
The cell load should be applied taking 1 minute to reach the prescribed level and
that level should be held for 2 minutes.
• Reduce the load to zero and remove the cell.
• Clean up the smaller opening sieve and pan, weigh the pan (Wp) accurately.
• Stack the smaller opening sieve on the pan and transfer all the cell contents onto
the sieve using the sieve brush.
• Place the sieve and pan on the sieve shaker and sieve for 10 minutes.
35
• Remove the sieve stack after sieving. Weigh the crushed materials with the pan
(W T) accurately.
• Calculate, as a percentage, of the crushed materials to the weight of 40g.
Calculation
W = W T - WP
wt% = W/40 × 100
Stress to be Applied and Suggested Maximum Fines for Fracturing Sand Crush
Resistance Tests
Mesh Size Load Stress Suggested Max. Fines
(lb force) (psi) (wt%)
6/12 6283 2000 20
8/16 6283 2000 18
12/20 9425 3000 16
16/30 9425 3000 14
20/40 12566 4000 14
30/50 12566 4000 10
40/70 15708 5000 8
70/140 15708 5000 6
36
Perrier14570 Hydraulic Press for Fracturing Sand Crush Resistance
37
HF-016 Crush Resistance Test (Testing RCP)

Introduction
It is currently a best practice to control the proppant flowback by placing RCP
proppant in the last fracturing stages in the field. The performance of the curing
properties of the used RCP is somewhat determining the job quality. A reliable lab
testing procedure is very helpful with regard to this RCP performance. Following
procedure is used for most RCP suppliers/manufacturers.
The objective of this testing is determining the bond strength of curable resin-coated
proppant at simulated downhole conditions.

---Hydraulic load frame: Carver laboratory press or equivalent capable of applying
3,000 psi on the test specimens. This equipment is used to break the test
specimens.
---Specimen mold: diameter/length ratio of 1:2.5 or greater, capable of maintaining
constant load on the specimen for the duration of the curing time, see attached
drawings or equivalent. For curing without stress @ atmospheric pressure,
polypropylene test tubes may be used, if sized appropriately.
---Heat source: capable of maintaining temperature ± 1°C [2°F] on the specimen
mold. A water/oil/sand bath or a forced draft laboratory oven, may be used as a
thermostated heat source.
---Saw: suitable for assuring that the cured slug ends are parallel and for dividing
long slugs into 2 or more test slugs.
---Deionized/distilled water
---Potassium chloride, ACS Reagent grade
---Curable resin coated proppant, as appropriate
---Mold release agent, silicone oil or equivalent
---Miscellaneous labware
Procedure
Cured Slug Preparation
1. Prepare curing media as appropriate. Curing media is normally 2% KCl in
deionized water.
2. Add curable resin coated proppant to the curing media. A widely used loading of
proppant is 6 lb/gal, added. Any loading of proppant may be used, however that
38
loading must approximate the actual job design expected. About 18 lbm/gal is a
practical limit.
3. Be sure the proppant is well dispersed in the liquid curing media. All entrained air
bubbles should be dissipated for best result, entrained air bubbles don't exist
downhole under pressure and they will weaken the cured slug. Use a good
wetting agent, if the bubbles will not dissipate with gentle stirring or swirling.
Filling the Molds

4. Load at least 3, preferably 6 specimen molds with sufficient wet proppant to give
a length of 2.5 times the diameter of the finished slug. Loading the molds must
occur before initial agglomeration of the proppant grains begins, but never longer
than 30 minutes after initial slurry preparation. For a diameter of 1inch [2.54 cm]
this would be about 2.5 inches long of proppant in the mold.
5. Be sure to tap the mold on the bench top or appropriate surface to eliminate air
bubbles and facilitate closest packing of the proppant in the mold.
6. Fill the porosity of the proppant in the mold with liquid cure media so that the top
surface is below liquid level. It is very important that the proppant be completely
submerged in the liquid cure medium.
7. Insert the piston, close the mold and apply gas pressure/closure stress to the
proppant in the mold. A widely accepted stress value is 1,000 psi [6,895 kPa] or
785 lbf [3,492 N] on a 1inch [2.54 cm] diameter slug. When using the suggested
apparatus the liquid valve is left open during the application of stress, then closed
during the application of temperature. For best results, the pack of proppant must
be under stress during the cure process. Separate experiments must be
performed, if you wish to investigate the effects of various closure stress levels or
stress ramping.
Curing the Test Specimens

8. Apply heat. The temperature should be maintained within ± 1°C [2°F] for the
duration of the cure time. As test temperature is approached near to the fluid
valve on the mold, close the fluid valve. Closing the valve too soon may generate
enough pressure, as the cell is heating, to prevent/reduce the intended closure
stress applied to the proppant slug. Closing the valve too late may allow loss of
too much fluid from the slug via evaporation or boiling.
9. Maintain temperature & stress during the cure time. Stress should be
maintained ± 10%.
10. Minimize stress fluctuations during the test.
39
11. At the end of the cure time release the stress and remove the cured slug from
the mold while the slug is still hot. Wear insulated gloves to prevent burns. Use
of the load frame to remove the slug from the mold requires careful attention and
skill. Do NOT apply undue stress to the slug during the removal process. Be
sure to use an effective mold release agent the next time.
12. Assure that the ends of the slug are parallel, and the length to diameter ratio, L/D,
is at least 2. A carbide masonry blade in a power table saw is recommended.
Use the piece guides. A carbide grinding wheel may be used with the proper jig
& safety equipment. A flat file may be used. The relatively soft upper end of the
slug must be removed.
13. Dry the prepared slugs. Air drying at ambient conditions for 24 hours should be
sufficient. Do not dry in an oven as temperatures above about 49°C [120°F] will
tend to further cure the resin coating giving misleading results.
Compressive Strength Measurement

14. Record the length & diameter of the test slugs. Average length & diameter are
used in calculations.
15. Place the prepared & dried slug in the load frame. Load frame should be
calibrated at least once each year, against traceable standards in compression
mode.
16. Close the platens on the slug. Do Not apply stress. The platens must be parallel
to within 0.005".
17. Begin applying stress to the slug. Apply stress at the rate of 4,000 lbf/minute.
For slugs with compressive strength less than 500 psi, use a loading rate of 1,000
lbf/minute.
18. Record the load required to break the slug. This number is pounds force or load,
Fg.
Calculations
19. Calculate the compressive strength of each slug.
Compressive Strength, Fc, psi = 4 x Fg/{(p x d²)[0.88 + (0.24d/h)]}
where: Fg = gauge reading, lbf

d = diameter of the slug, inch
h = length of the slug, inch
40
Note: [0.88 + (0.24d/h)] is an h/d correction for test specimens which have
ratios < 2, from ASTM D2938. The correction becomes unity (zero effect) at
h/d = 2. The correction is not used when h/d > 2.
20. Average the values for all the slugs.
41
Reporting
21. Report all test conditions. Report, cure temperature & time, closure stress during
curing, curable proppant size & type, all test specimen dimensions (diameter &
length), force at failure for each slug, calculated compressive strength, averages
& the standard deviation.
Schematic Diagram of Testing Equipment
42
HF-017 Proppant Acid Solubility Test (API RP56)

Introduction
The solubility of sand in 12-3 hydrochloric-hydrofluoric acid (HCl-HF) (that is, 12
percent by weight of HCl and 3 percent by weight of HF) is an indication of the
amount of undesirable contaminants (for example, carbonate, feldspars, iron oxides,
clays) present in sand.
The API recommended maximum acid soluble material content in fracturing sand is
2.0wt% for 6/12 through 30/50 and 3.0wt% for 40/70 through 70/140.
Apparatus and Materials
Weighing balance to 0.0001g
Waring blender with mixing cup
Oven
Dessicator
Water bath
Beaker or jar, 150-200ml, polyethylene or polypropylene
1000ml volumetric flask, polyethylene or polypropylene
Water suction pump
Whatman membrane filter holder, fritted glass support, 300 micron capacity
Membrane filter, cellulose nitrate, white plain, 47mm, pore size 0.4 micron
50ml/25ml Gooch crucible and Whatman 40 filter paper
1 liter filtering flask fitted with buchner funnel and rubber sleeve
12-3 (wt%) HCl-HF acid solution
Split sand sample
DI water
Test Procedures
• Preparation of Gooch Crucible filter paper pulp
Measure 900ml DI water in a waring blender. Tear 2 pieces of Whatman #40 filter
papers into small pieces and place them into water. Blend the mixture at high
speed for 1 minute. A paper pulp will be obtained. Pour the pulp slurry full into a
50ml/25ml Gooch crucible. Place it in a buchner funnel with a rubber sleeve
sitting on a 1-liter filtering flask. Switch on the vacuum pump and drain out the
slurry with filter paper pulp remaining at the bottom covering the crucible holes.
Dry the crucible in a oven at 100oC for 2 hours and store it in the dessicator for
acid solubility use.
• Preparation of 1000ml 12-3 (wt%) HCl-HF solution
43
Add 46.23g pure NH4HF2 to 500ml DI water contained in the 1000ml polyethylene
flask and dissolve. Add 361ml of 37% HCl. Dilute with DI water to 1000ml and stir
to ensure complete mixing.
• Weigh accurately 5g of dry sand sample (W1) into the 150/200ml plastic beaker
containing 100ml of 12-3 HCl-HF acid solution.
• Cover the beaker with watch glass and place it into the water bath at 65.6oC for
30-35 minutes. Do not stir it.
• Weigh the crucible with filter paper pulp accurately. (W2)
• Transfer the sand-acid mixture from the beaker to the filtering apparatus. Filter
the sample through the pre-weighed crucible being sure all solids are filtered.
Flush the beaker with DI water three time to get all samples being filtered.
• Dry the filter with retained sample at 100oC for 2 hours. Cool the filter and sample
down in a dessicator.
• Weigh the crucible with the retained sample accurately. (W3)
• Calculate the report percent acid solubility.
Calculation
S = (W1 + W2 – W3) × 100 / W1
Where:
S, acid solubility, wt%
W1, sample weight, gram
W2, weight of filter, gram
W3, weight of filter containing sand sample, gram
44
SECTION 2 MATRIX ACIDIZING
Introduction
Procedures 02-001 to 02-014 describe formulation and properties of most-used
matrix acidizing systems in Schlumberger well services.
The acids are based upon 36% hydrochloric acid. All formulations make 1,000
milliliters.
Safety
Goggles, rubber gloves and a protective covering must be worn when mixing acids.
Always work under a fume hood when preparing acids.
ALWAYS ADD CONCENTRATED ACID TO WATER.
Glass and Plastic graduated cylinders
Funnels
Labels for containers
Most Used Acid Systems in Schlumberger Well Services
Major Application Acid Systems
Carbonate Acidizing Hydrochloric Acid
Intensified Acid
Sandstone Acidizing Mud Acid
Clay Acid
Organic Mud Acid
Organic Clay Acid
Gas Well Alcoholic acid
Gas Well Acid
Gas Well Mud Acid
Retarded Acid DAD acid
SXE/SXE HT
Gelled Acid LCA/SDA/VDA
Mud Removal BDA
MSR
NARS
Organic Damage Removal CLEAN SWEEP
Scale Dissolving CAS U104/U105/U106
Perforating Acid Aqueous Acetic Acid
Formic Acid
Perforating acid
45
MA-001 Hydrochloric Acid Laboratory Preparation

Hydrochloric acid is a solution of HCl gas in water. Maximum concentration of
commercial acid product is 36%. Following table lists mostly-used hydrochloride
acids in oilfield industry.
Refer to following table to prepare 1000ml HCl different diluted acid from 36%
concentrated one. The mass balance should be applied for the calculation is
Volume of diluted acid × Density of diluted acid × Acid strength of diluted acid =
Volume of concentrated acid × Density of concentrated acid × Acid strength of
concentrated acid
Dilutions of Concentrated Hydrochloric Acid

HCl Acid Strength 36% HCl needed (mL) Density (g/cc)
28% 751 1.141
20% 507 1.099
15% 379 1.074
10% 247 1.049
7.5 % 183 1.036
5.0% 120 1.024
Mixing Procedures
To prepare 1,000mL of HCl:
• Place some amount of water in 1000ml volumetric flask.
• Add the required quantity of concentrated HCl into the flas very slowly. Heat and
smell will be released during the preparation, it is strongly recommended to
operate in fume hood.
• Top up the flask to graduated line (1000ml).
• Shake the capped flask a few times of upside down.
46
MA-002 Intensified Acid

Intensified acid is a regular inhibited HCl (generally 15%) with addition of 33.8
lbs/Mgal Y001 (0.25%). It is generally used in initial cleanup as well as in dolomitic
limestone containing certain amount of silica. As high as 50% more reaction of
intensified acid and dolomitic limestone increases at surface conditions. The increase
is less pronounced at elevated temperature. Field results also confirm the value of
intensified acid as a cleanup treatment in dolomitic limestone formations.
CaF2 precipitates is the side reaction product to have potential damage by intensified
acid treatment.
Mixing procedures
(1) Use plastic beaker to contain HCl base acid with required amount of inhibitor.
(2) Stir the solution to homogeneous by magnetic stirrer.
(3) Add required amount of Y001 (33.8lb/Mgal) slowly.
(4) Stir the mixture until a clear solution being prepared.
47
MA-003 Clay Acid Laboratory Preparation

Clay acids are designed for sensitive sandstone matrix stimulation. It slowly release
HF from the hydrolysis of HBF4 so that the acid can penetrate further into the matrix
than mud acid.
Four types of clay acids are generally used, they are full strength clay acid, full
strength clay acid LT, half strength clay acid and half strength clay acid LT. Clay
acids are generally used in temperature range of 130F-300F, but clay acids LT are
only used for the temperature range of 100F to 130F.
In order to prepare Clay Acid properly the additives must be added in the order listed,
otherwise a precipitate will form. Each formulation prepares 1000 mL of Clay Acid.
Note: Y006 and L010 have the same composition and can directly replace each
other.
Clay Acid
Full Strength Clay Acid H813 Half-Strength Clay Acid, H913
Water 680 mL 843 mL
Y001 120 g 60 g
35% HCl 194 mL 97 mL
Y006 60 g 30 g
S.G. 1.096 1.047
Low Temperature Clay Acid

Full Strength Clay Acid LT Half-strength Clay Acid LT, H914
H814
Water 545 mL 772 mL
Y001 120 g 60 g
35% HCl 336 mL 168 mL
Y006 60 g 30 g
S.G. 1.121 1.047
48
MA-004 Mud Acid Laboratory Preparation

Mud acid is a mixture of inhibited HCl acid and hydrofluoric acid. Due to the safety
issue of concentrated HF acid, it is strongly recommended to mix the mud acid with
Y001 listed in the following table.
Not only dissolving the minerals which HCl acid can dissolve, Mud acid can also
dissolve siliceous minerals presented in most sandstone formations.
It is always noted that Calcium/Magnesium/Sodium/Potassium brines can react with
HF acid to form insoluble precipitates.
The table below contains volume required to prepare the most common Mud Acid
formulations.
Mud Acid Formulations
Concentration 36% HCl Y001 Water Density
mL g mL g/cc
4% HCl - 0.5% HF 110 7.2 885 1.022
6% HCl - 0.5% HF 160 7.2 835 1.032
8% HCl - 0.5% HF 210 7.2 785 1.041
6% HCl - 1 % HF 170 15 820 1.036
8% HCl - 1 % HF 220 15 770 1.045
10% HCl - 1 % HF 270 15 720 1.054
6% HCl - 1.5% HF 180 24 804 1.041
7.5% HCl - 1.5% HF 220 24 764 1.048
10% HCl - 1.5% HF 290 24 694 1.061
12% HCl - 1.5% HF 340 24 644 1.07
10% HCl - 2 % HF 300 30 680 1.065
12% HCl - 3% HF 380 48 588 1.085
Mixing Procedures
WEAR SAFETY GOGGLES, PROTECTIVE CLOTHING AND RUBBER GLOVES.
WORK IN A FUME CUPBOARD.
• Place appropriate quantity of fresh water in a plastic beaker. Do not use sea
water, oilfield brine, calcium, magnesium, potassium or sodium chlorides to
prepare Mud Acid.
• Add required amount of Y001. Mix using a magnetic stirrer until the Y001 has
dissolved completely.
• Add the required quantity of concentrated HCl slowly. Mix until clear. (Note: Heat
Will Be Generated!)
49
MA-005 Oganic Mud Acid Preparation

Organic mud acid is a mixture of 9% formic acid (L36) and 3% hydrofluoric acid. It is
easier to be inhibited, has lower reaction rate and less tendency to form asphaltic
sludge.
It is recommended to use for high temperature matrix acidizing and wellbore damage
removal in both sandstone and carbonate reservoirs where extended inhibition time
is expected and asphaltic sludges are formed when contacted with HCl acids.
BOTH Y001 AND L36 CAN CAUSE SEVERE EYE AND SKIN BURNS, WEAR
PROPER PPE
Mixing procedures
• Add certain amount of fresh water in the plastic beaker. Stir with magnetic stirrer
to Votex.
• Add A186 as required to mix thoroughly.
• Add required Y001 into the beaker slowly, stir until totally dissolved.
• Add required amount of HCl acid and L36.
• Top up the container to total volume with fresh water.
• Formulation for preparing 1000ml as follows
---Fresh water
---Inhibitor as required
---48g Y001
---72ml 36% HCl
---90ml L36
50
MA-006 Oganic Clay Acid Preparation

Organic Clay Acid system is designed for acidizing sandstones containing high
silt/clay content and HCl sensitive formations. It is helpful in reducing secondary
precipitation and fines migration after the treatment. It can remove formation
damages by clay and other aluminosilicate minerals and be used for high
temperature applications.
Following tables list two OCA formulations (OCA-R and OCA-HT) and their
application conditions. The addition sequence as indicated in the table.
Component OCA-R OCA-HT
HCl+inhibitor 5% 1.5%
J285 5% 5%
L001 13.4% 10%
Y001 5% 2%
Y006 2.5% 1.2%
Conditions OCA-R OCA-HT

>300F - *
<300F, silt/clay>30% * -
>5% zeolite - *
<5% zeolite * -
>5% chlorite - *
<5% chlorite * -
* fluid applicable
51
MA-007 Alcoholic Acid Laboratory Preparation

Alcoholic acid is a mixture of acid (HCl or mud acid) and alcohol (F003 or K046).
The effects of adding alcohol into the acid are
(1) lower the surface tension.
(2) Increase the vapor pressure and improve post cleanup effectiveness.
(3) Retardation of the acid reaction rate and offer improved success in acidizing low
to medium permeability dry gas formations.
(4) Corrosion rate is slightly accelerated by the addition of alcohol in acid.
The concentration of alcoholic acid mixtures indicates the volume percentage of each
additive in the acid. For example, an 80:20 alcoholic acid mixture is prepared by
mixing 800 ml of acid (e.g. 15% HCl) and adding 200 ml of alcohol. Note, when the
above mixture is prepared there is a volume loss of 10 ml.
52
MA-008 Gas Well Acid Laboratory Preparation

Introduction
Gas Well Acid is 15% HCl prepared by diluting concentrated HCl with Methanol
K046. Isopropyl alcohol, F003, cannot be substituted for K046. The only amount of
water present in15% Gas Well Acid is the small quantity of water present in the
concentrated acid. Thus, there is limited water available to solubilize or disperse
additives. Additives soluble in methanol or other pre-tested additives can be used.
These must be tested in the lab.
Mixing Procedures
To prepare 1,000 ml of Gas Well Acid
• Add K046 and appropriate amount of corrosion inhibitor, A261 for a total volume
of 670 mL in a dry beaker.
• If confirmed by lab tests (compatibility tests), add W-agent, iron stabilizer and
other additives to the beaker.
• Add 330 ml of concentrated HCl and mix using a magnetic stirrer. A rise in
temperature, caused by dissolving heat, is normal.
• If specified by lab testing, appropriate additives may be added at this stage. Label
the container appropriately.
53
MA-009 Gas Well Mud Acid Laboratory Preparation

Introduction
Gas Well Mud Acid contains 8% HCl and 3% HF acid (by weight) plus K046
Methanol. The Table below contains the loading schedule for Gas Well Mud Acid
prepared using concentrated HCl, Y001 Intensifier and fresh water.
Gas Well Mud Acid Using Conc. HCl and Y001
Concentrated HCl Volume K46 Volume Y001 Fresh Water Volume
Acid Strength (ml) (ml) (g/l) (ml)
28% HCl 315 532 42 120
29% 303 544 42 120
30% 292 555 42 120
31% 281 566 42 120

32% 271 576 42 120
33% 262 585 42 120
34% 253 594 42 120
35% 245 602 42 120
36% HCl 237 610 42 120
Mixing Procedures
To prepare 1,000 ml of Gas Well Mud Acid:
• Place the required amount of water to prepare the Mud Acid in a plastic beaker.
• Add the required amount of Y001 to generate the Mud Acid formulation. Y001 will
cool down the water.
• Add the required amount of A261 Corrosion Inhibitor. If supported by lab tests,
add W-agent, iron stabilizer and other additives.
• Add the concentrated HCl and mix using a magnetic stirrer for 3 minutes.
• Add the K046 Methanol. Mix for 3 minutes.
If specified by lab testing appropriate additives may be added at this stage. Label the
container appropriately.
54
MA-010 Dowell Acid Dispersion (DAD)

Introduction
Dowell Acid Dispersion is an acid outside-phase emulsion stabilized with Dispersing
Agent U074. The purpose of the dispersion is to simultaneously dissolve the minerals
and remove the oily paraffinic deposits.
The dispersion can be prepared with various acids and hydrocarbon solvents. Most
common are HCl and P121 (toluene). Ratios of acid: hydrocarbon can be made from
10 to 50%. Usually 15 gallons of U074 per 1000 gallons of acid is used to stabilize
the emulsion.
Mixing Procddures
• Prepare 450 ml of 15% HCl acid. Add appropriate corrosion inhibitor for suitable
protection time.
• Place 50 mL of P121 in a Waring blender cup. Add the required quantity of U074.
The resultant volume should be 50 mL plus volume of U074.Create a vortex
down to the blades of the blender. Mix for 3 minutes.
• Note: The fumes are hazardous. Prepare the DAD under a fume hood or use
appropriate precautions.
• Continuing mixing. Slowly add a volume of acid through the hole in the blender
cup lid equal to the volume of solvent /U074 mixture prepared in the second step.
• Increase the speed of the Waring blender to around 1,000 rpm. Mix for 10
minutes. At this time an oil-outside phase dispersion should form. The fluid will
have some viscosity and may stick to the sides of the blender cup. This is the
“seed batch” dispersion.
• Continuing mixing as Step four, slowly and at a steady rate, add the acid solution
through the hole in the blender lid to the seed batch. The emulsion should invert
to become acid outside phase. The fluid should wet the sides of the blender cup
and easily drain down the sides of the cup.
• Mix for a further 15 minutes at 1,000 rpm.
• The DAD will be stable for the times quoted in the MMM. It cannot be stored for
long lengths of time.
55
MA-011 Demonstrating Crosslink of Leak-off Control Acid or Self- Diverting Acid
Introduction
This method describes the preparation of Leak Off Control Acid (LCA)* as well as a
method to demonstrate the crosslinking affect of the LCA during reaction with
calcium carbonate. The latter represents a carbonate formation such as limestone or
dolomite. LCA utilises gelling agents to thicken 15%, 20% or 28% hydrochloric acid.
Reference should be made to the Matrix Materials Manual section 130.30.
Note: LCA is also known as Self Diverting Acid (SDA)
Safety
Hydrochloric acids solution are extremely corrosive and HCl vapors are toxic.
Ensure eyes and hands are adequately protected. The HCl vapors should be
avoided and handling should be performed in a fume cupboard or well-ventilated
area.
The gelling agents used to prepare LCA fluids may cause permanent damage if
exposure to the eye occurs. Again protect eyes and hands while handling.
All personnel should be thoroughly acquainted with potential hazards of the reagents,
products and solvents to be utilised in a procedure before beginning work. Always
consult the Dowell Material Safety Data Sheets before using the chemicals.
Waring Blender
Blender Cup, 1 Litre
Disposable Syringes, 5 and 10 mL
Large Beaker, 2 L
pH Meter or Paper
Fann 35 Viscometer
Magnetic Stirrer or Overhead Stirrer
J429/J476C/(J507) Acid Gelling Agents (J507 for North Sea)
J471A Iron Control Agent
J472 Fluid Loss Additive
A166(A262) Corrosion Inhibitor (A262 for North Sea)
A201 Corrosion Inhibitor Aid
Consult the Dowell Matrix Materials Manual, Section 130.30 to determine quantity of
corrosion inhibitors required.
56
Mixing Procedures
• This procedure concentrates on a specific acid design to demonstrate the

crosslinking of the LCA. A similar method can be used for all concentration of HCl
and additives used to prepare LCA.
For example to prepare 500 mL of LCA using 15 % HCl (LCA 15)
481 mL H015 15%HCl acid
10 mL J429 Acid Gelling Agent
5 mL J471A Iron Control Agent
2.5 mL J472 Fluid Loss Agent
2 mL A166 Corrosion Inhibitor
• Preparation of LCA
--- Add 481 mL of 15% HCl to the Waring cup. With the blender running at a
speed to create a vortex down to the blades. Add 2 mL ofcorrosion inhibitor.
--- Continuing mixing, slowly add the 5 mL ofJ471A.
--- Add 2.5 mL of J472. Mix until completely dispersed, approximately one
minute.
---Add the 10 mL of the gelling agent (J429, J476C or J507) at a slow, constant
rate to the edge of the vortex.
--- Mix at 1000 rpm for 5 minutes.
--- Measure the viscosity of the fluid using the Fann 35 Viscometer. Viscosity at
75°F (24°C) and 170 sec-1 (100 rpm) should be 48 to 60 cP.
• Crosslinking of LCA
This part of the procedure demonstrates the spending of the LCA 15 using
calcium carbonate to induce the crosslinking of the LCA fluid.
--- Place 400mL LCA in a 2000 mL beaker.
--- Start mixing at slow speed using an overhead stirrer or a magnetic stirrer.
--- SLOWLY add fine grade calcium carbonate (60-150 micron e.g. IDCARB 150)
in small batches of around 10 grams, because the reaction is STRONG.
--- Take care to spread each batch of the CaCO3 evenly over the surface of the
gel. Extensive foaming will occur. You will need 70 - 80 grams of CaCO3 to spend
the 400mL of LCA.
--- Measure the viscosity and pH after each addition of calcium carbonate on a
Fann 35 viscometer at 170 sec-1. You will visually see the LCA viscosity start to
increase due to the increase in pH.
57
--- Increase the speed of mixing as the fluid gets thicker. If you do not have an
overhead stirrer the CaCO3 can be mixed in by hand using a plastic spatula.
TAKE CARE.
--- When the pH reaches 4.4 - 4.8 the fluid should be fully crosslinked and
resemble a ball of thick gel. At this time you will not be able to measure the
viscosity of the gel using the Fann 35 Viscometer, as the gel will “climb” the bob,
making a steady reading impossible.
• An example of the results from a crosslink test are shown below:
CaCO3 Viscosity pH
(g) cP, (@170sec-1)
0 60 0 - 0.5
25 90 0 - 0.5
35 90 0 - 0.5
45 90 0 - 0.5
55 96 0 - 0.5
65 99 1.5
75 150* 5.5
58
MA-012 Breakdown Acid (BDA) Laboratory Preparation

Introduction
BDA acid is designed primarily to open or breakdown the target interval prior to a
fracturing or matrix acidizing treatment. This acid will lower the breakdown pressure
and provide better coverage of the perforated interval. The principle of this capacity is
from the dispersion and suspending capacity of surfactant F078.
Norammly BDA acid is 7.5 or 15 % HCl acid containing 5 gal F78 per 1000 gallons of
acid.
Mixing procedure
• Add certain amount of mix-water in the beaker.
• Add required amount of inhibitor to mix thoroughly.
• Add 5ml of F078 into the solution to mix completely.
• Add required amount of concentrated HCl and top up to 1000ml by the mix-water.
59
MA-013 Mud Silt Remover Acid (MSR) Laboratory Preparation

Introduction
MSR is an acid solution containing a clay dispersant-suspending agent and an iron
chelating agent. Combination of this two additives provides not only good dispersion
of drilling muds and silt/fines from formation, but also an effective suspension
properties.
MSR applications include removal of mud damage, use as a workover fluid to restore
fracture conductivity or use as a breakdown or matrix treatment fluid to open clogged
perforation or restore the permeability.
There are three distinct formulations: MSR100, MSR150 and MSR123.
Compositions of MSR Formulations
Agent MSR100 MSR150 MSR123
L41 12 g 18 g 6g
(or U42) (20 ml) (30 ml) (5 ml)
F78 5 ml 5 ml 5 ml
U66 - - 100 ml
Carrier Fluid 7.5% HCl to 15% HCl 7.5% HCl to 15% HCl Mud Acid
(12% HCl + 3% HF)
(or 3% NH4Cl, 2% KCl) (or 3% NH4Cl, 2% KCl)
Mixing Procedures
To prepare 1,000 ml of MSR:
• Prepare the appropriate acid concentration using the procedures for HCl or Mud
Acid.
• Place 200 ml of acid in a plastic container.
• Add the appropriate quantities of the additives as listed in above table.
• Make the solution up to 1,000 mL using the remaining acid solution.
60
MA-014 Non-Acid Reactive Solutions

Introduction
NARS systems are mainly used for “acid-sensitive” formations, which generally
poorly developed sandstones and dolomites with large amounts of silt and shale.
These minerals can be partially decomposed by low pH fluids to form silica gel to
further damage the formation.
The chelating agents contained in NARS systems can dissolve or partially dissolve
the sandstone minerals. The mutual solvent inside the system enhance the water-
wetting property. The surfactant combination with chelating agent provides an
optimum dispersion of clays for suspension and removal. The clay stabilizer will
suppress the clay movement.
No inhibition is needed for NRAS systems and recommended for high temperature
applications.
Mixing Procedures (as listed in following table)
Mixing order of 1000ml NARS systems

Order of addition Materials NARS200 NARS201
1 Fresh water 600ml 600ml
2 U042 50ml 50ml
3 M117 20g 20g
4 U066 100ml 100ml
5 F078 5ml ---
F075N --- 5ml
6 L055 --- 5ml
7 fresh water Top up Top up
61
MA-015 CLEAN SWEEP Fluids Laboratory Preparation

Introduction
CLEAN SWEEP fluids are multifunctional solvents used primarily to remove water
blocks and restore the relative permeability of the reservoir to oil and gas. Paraffin
solvent, mutual solvent and water-free acid are the key components to dissolve
paraffin deposits, decrease the in-place-oil viscosity, reduce surface or interfacial
tension, break emulsions, dissolve scales and even other iron-bearing minerals.
Mixing Procedures
Following table lists the formulation of different CLEAN SWEEP fluids and the order
of additive addition in preparing each fluid.
Additives in 1000ml CLEAN SWEEP fluid
Component CLEAN SWEEP I CLEAN SWEEP II CLEAN SWEEP III
A026 800ml --- ---
P121 --- 800ml ---
K046 --- --- 800ml
U066 100ml 100ml 100ml
L400/L401 100ml 100ml 100ml
A186 added at 1 ml
Any extra water contamination will cause phase separation
62
MA-016 Aqueous Acetic Acid Laboratory Preparation

Introduction
The primary advantages of acetic acid is offering extended exposure time at elevated
temperature and providing slow reaction rate with carbonate rocks and minerals in
addition to controlling the clay migration and iron precipitates by buffering the solution
pH.
Preparation
Aqueous acetic acid is prepared using either glacial acetic acid (L400) or low freezing
point acetic acid solution (L401). Commonly 10% acetic acid is used. Following table
lists common acetic acids diluted from L400 or L401. Add inhibitor first for the mixing.
Always add the acetic acid to the water.
Acetic Acid Dilution

Acetic Acid Specific Gravity ml of L400 for ml of L401for
Concentration (20 deg C) 1000 ml Solution 1000 ml Solution
2% 1.0012 19 26
3% 1.0025 25 39
4% 1.0040 38 52
5% 1.0055 48 65
6% 1.0069 58 78
7% 1.0083 67 91
8% 1.0097 77 104
9% 1.0110 87 117
10% 1.0125 97 130

11% 1.0139 106 144
12% 1.0154 116 157
63
MA-017 L036 Laboratory Preparation

Introduction
L036 is a mixture of inhibited formic acid diluted in water, which is generally used to
stimulate oil and gas wells. The acid strength is between that of HCl and acetic acid.
It reacts slowly with carbonate formations and many minerals presented in
sandstone. Maximum L036 concentration for treatment is 9%. Higher concentrations
may cause insoluble calcium formate precipitate.
Mixing Procedures (for preparing 1,000 ml of 9% L036)

• Mix the water and additives (corrosion inhibitor/mutual solvent/surfactant
confirmed by compatibility tests) to produce a volume of 910 ml
• Slowly add 90 ml of concentrated L036. Thoroughly mix to obtain a uniform
solution.
• Correctly label the container.
• To prepare a more dilute concentration, use 10 ml of L036 for each percent of
desired concentration to make 1,000 mL of final mixture.
64
MA-018 HCl Acid Strength Test

Introduction
A titration method is used to determinee the HCl acid strength. An equation is
attached in the calculation section for adjusting the acid concentration.
0.5 ml Pipette
20ml Buret
Conical Klask (25-50ml)
DI water
0.5N NaOH standard solution
Unknown conc. of HCl
Phenolphthalein indicator
Procedure
• Clean the conical flask with DI water for three times.
• Pipette 0.5ml of HCl solution into conical flask. Flush the flask wall with about 5ml
of DI water to get all acid into the solution.
• Add 2-5 drops of phenolphthalein indicator into the solution and shake to
disperse.
• Titrate the acid with 20ml Buret containing 0.5N NaOH standard solution until the
color change to pink.
• Record the mls of NaOH solution used (A ml).
• Repeat the above procedures for three times.
Calculation
• Molarity of HCl acid = A mol/l
• See the conversion table for wt% of HCl
• Equation for adjusting the acid strength
Volume of strong × S.G. of strong × wt% of strong = Volume of dilute × S.G. of dilute
× wt% of dilute
65
S.G. – Weight concentration – Molority Relationship of HCl Acid
HCl conc.(wt%) S.G. Molority (mol/l)

1 1.0048 0.2753
2 1.0097 0.5533
3 1.0147 0.8340
4 1.0197 1.1175
5 1.0248 1.4038
6 1.0299 1.6930
7 1.035 1.9849
8 1.0402 2.2799
9 1.0447 2.5760
10 1.05 2.8767
11 1.055 3.1795
12 1.06 3.4849
13 1.0646 3.7917
14 1.0702 4.1049
15 1.0749 4.4174
16 1.0801 4.7347
17 1.0849 5.0530
18 1.0902 5.3763
19 1.0952 5.7010
20 1.1002 6.0285
21 1.1057 6.3616
22 1.1108 6.6952
23 1.1159 7.0317
24 1.1214 7.3736
25 1.1261 7.7130
26 1.131 8.0564
27 1.1368 8.4092
28 1.1422 8.7621
29 1.1471 9.1139
30 1.1526 9.4734
31 1.1577 9.8325
32 1.1628 10.1944
33 1.168 10.5600
34 1.1727 10.9238
35 1.1779 11.2949
36 1.1827 11.6650
37 1.188 12.0427
66
wt% -SG-Molority of HCl

1.25 14.00
1.20 12.00
1.15 10.00
Molority (mol/l)
1.10 8.00
S.G.
1.05 6.00
1.00 4.00
0.95 2.00
0.90 0.00
1 5 9 13 17 21 25 29 33 37
weight concentration (wt%)
67
MA-019 Acid Solubility Test

Introduction
The solubility of scale or formation sample in 15% HCl or 15% HCl followed by RMA
(that is, 12 percent by weight of HCl and 3 percent by weight of HF) is an indication
of the amount of carbonate and clay minerals presented in the tested sample. A
weighed sample is treated with acid, the insolubles are filtered out and weighed. The
amount of disolved then can be determined from the difference between the sample
weight and residue weight.
Weighing balance to 0.0001g
Waring blender with mixing cup
Oven
Dessicator
Water bath
Beaker or jar, 150-200ml, polyethylene or polypropylene
1000ml volumetric flask, polyethylene or polypropylene
Water suction pump
Whatman membrane filter holder, fritted glass support, 300 micron capacity
Membrane filter, cellulose nitrate, white plain, 47mm, pore size 0.4 micron
50ml/25ml Gooch crucible and Whatman 40 filter paper
1 liter filtering flask fitted with buchner funnel and rubber sleeve
15% HCl
12-3 (wt%) HCl-HF acid solution
about 1g formation sample (sieved under US sieve #40)
DI water
Test Procedures
A) solubility in 15% HCl (wash sample with toluene first if it contains hydrocarbons)

sitting on a 1-liter filtering flask. Switch on the vaccum pump and drain out the
slurry with
68
filter paper pulp remaining at the bottom covering the crucible holes. Dry the
crucible in a oven at 100oC for 2 hours and store it in the dessicator for acid
solubility use.
• Weigh accurately about 1g of dry pulverized sample (W1) into the 150/200ml
plastic beaker containing 100ml 15% HCl acid. Mix and disperse the powder
sample in acid.
• Cover the beaker with watch glass and place it into the water bath at 65oC for 60
minutes. Swirl the beaker occasinally.
• Weigh the crisible with filter paper pulp accurately and the piece of filter paper.
(W2)
• Transfer the sample-acid mixture from the beaker to the filtering apparatus. Filter
• Filter the filtrate through the membrane filter paper.
• Dry the crucible and filter paper with retained sample at 100oC for 2 hours. Cool
them down in a dessicator.
B) Solubility in 15% HCl followed by RMA(wash sample with toluene first if it

contains oil)

sitting on a 1-liter filtering flask. Switch on the vaccum pump and drain out the
slurry with filter paper pulp remaining at the bottom covering the crucible holes.
Dry the crucible in a oven at 100oC for 2 hours and store it in the dessicator for
acid solubility use.
• Preparation of 1000ml 12-3 (wt%) HCl-HF solution
Add 46.23g pure NH4HF2 to 500ml DI water contained in the 1000ml polyethylene
flask and dissolve. Add 361ml of 37% HCl. Dilute with DI water to 1000ml and stir
to ensure complete mixing.
69
• Weigh accurately about 1g of dry pulverized sample (W1) into the 150/200ml
plastic beaker containing 100ml 15% HCl acid. Mix and disperse the powder
sample in acid.
• Cover the beaker with watch glass and place it into the water bath at 65oC for 60
minutes. Swirl the beaker occasinally.
• After 1 hour, filter HCl through a new membrane filter but allow the residue to
remain in the plastic beaker.
• Wash down the residue sticking on the filter paper back to the beaker with the aid
of a washing bottle containing RMA.
• Top up the beaker to 100ml with RMA.
• Place the beaker containing sample and RMA in the water bath at 65oC for
another 1 hour.
• Weigh the crisible with filter paper pulp accurately and the piece of filter paper.
(W2)
• Transfer the sample-acid mixture from the beaker to the filtering apparatus. Filter
• Filter the filtrate through the membrane filter paper.
• Dry the crucible and filter paper with retained sample at 100oC for 2 hours. Cool
them down in a dessicator.
Calculation
S = (W1 + W2 – W3) × 100 / W1
Where:
S, acid solubility, wt%
W1, sample weight, gram
W2, weight of filter paper and crucible, gram
W3, weight of filter containing sample, gram
70
MA-020 Determination of Total Iron
Introduction
Total iron content in the formation powder can be determined by testing the iron
concentration in the filtrate after 15% HCl acid solubility test.
Hach 2000 Spectrophotometer and accessories
Volumetric flask, 500ml; 100ml
Pipette, 10ml
DI water
100ml filtrate from 15% HCl acid solubility test
Test Procedures
• The filtrate from 15% HCl acid solubility test is neutralized with ammonium
hydroxide to pH7 and then diluted to 500ml using 500ml volumetric flask.
• Pipette 10ml of solution from 500ml volumetric flask and place it into the 100ml
volumetric flask and dilute to 100ml.
• Switch on the HACH2000 Spectrophotometer.
• Enter the stored program number for iron (Fe, FerroVer powder pillows). Press
265 READ/ENTER.
• Rotate the wavelength dial until the small display shows 510nm.
• Press READ/ENTER. It will show: mg/l Fe.
• Pour 25ml of sample into the sample cell. Add the contents of one FerroVer Iron
reagent powder pillow to the sample cell (the prepared sample). Swirl to dissolve.
• Press SHIFT TIMER. Start reaction.
• When the timer beeps, fill another sample cell (blank) to 25ml of sample. Place it
into the cell holder and close the light shield.
• Press ZERO to zeroing the machine.
• After “ 0.00mg/l Fe ” shows up, place the prepared sample into the cell holder.
Close the light shield.
• Press READ/ENTER to get the reading in mg/l (A mg/l).
Calculation
Percentage of Iron in sample (wt%) = A / (2 × B) wt%
B, grams of sample used for 15% HCl acid solubility
71
MA-021 Acid Corrosion Inhibitor Evaluation

Introduction
Acid corrosion inhibitors are evaluated in terms of metal loss and pitting tendency
resulting from exposure to a given type of acid at varying concentrations,
temperatures and exposure times.
There is no standard testing procedure existing in the oil industry. So corrosion
protection claims published by various companies are generally not directly
comparable.
Testing up to 175 ºF can be carried out in a water bath under a fume hood but higher
temperature work requires the use of equipment such as a Parr Stirred Reactor
model 4521 (Hastelloy B) (see LEM Div II-N). Test procedures tend to be long and
the end result is only one point on a curve. For this reason and considering the semi-
quantitative nature of the results obtained, testing is perhaps best limited to
screening of “cheap local products” against accepted oil field products.
Ultrasonic bath
Water bath
Desiccator
Metal coupons
4-oz glass bottles with caps
4-oz caps fabricated with hooks
Disposable syringes
Tooth brush
DOWCLENE chlorinated solvent
Acetone
NOTE:
(1) Test up to 175oF. For temperatures above 175 ºF (dynamic tests), contact SHPC
for performing the test in a proper corrosion tester.
(2) Even if 2 3/8” OD N 80 oilfield tubing is used for all tests, it should be noted that
steel quality may vary considerably from one batch to another and even between
joints of the same batch. Thus, a variance in measured corrosion rate of 30-50
percent may arise.
(3) The tubing should be cut into 1” wide rings and the rings quartered with an oil-
cooled power band-saw. Test tubing protective coating, mill scale and rough
72
edges can be removed by drum rolling approx 250 coupons (5 ft tubing) in an

aluminium oxide-kerosene slurry. Identification numbers should then be stamped
onto the coupons.
(4) It is important to stress in any report that the test period refers to the time at test
temperature and does not include heat-up or cool-down. This can make a
significant difference for high temperature tests.
Test Procedures
• Place the coupons in an ultrasonic bath containing DOWCLENE chlorinated
solvent for 20 minutes, rinse in acetone, dry and then store in a dessicator until
required for use.
• Place 100 ml of acid into a 4 oz. Bottle. This volume of acid yields an acid
volume to coupon area ratio of 25 ml/inch2.
• Add inhibitor and any other additives for the system and shake to mix.
• Submerge a pre-weighted test coupon into the acid system preferably by
suspending it from a glass hook attached to the bottle cap.
• Place the bottle in a water bath at the test temperature and leave for the duration
of the test period. Record only the time at temperature, heat-up and cool-down
time should not be included.
• The coupons are then cooled, scrubbed with soap and a tooth brush, rinsed in
acetone, dried and reweighed.
Calculation
(1) Corrosion Rate
weight loss in grams × 2.048

Corrosion (lbs / ft2) =
coupon area in cm2
If a large number of tests are to be conducted with the same size and type of
coupons the calculations can be simplified to:
weight loss in grams × 2.048

Corrosion (lb / ft2) =
initial weight of coupons × F
Average area of coupons

where: F =
Average weight of coupons
73
The following limits have been set by DS as “acceptable”.
Temperature (ºF) Corrosion per test period

(lbs/sqft)
Up to 200 0.02
210 – 250 0.05
250 – 275 0.075
above 275 0.09
No recommended system should exceed these limits by 0.02 lb/ft2 maximum.
(2) Pitting tendency

Most pipe failures caused by acidizing are the result of concentration cells. Pipe near
such a cell may be completely undamaged but a single pit is all it take to cause a
failure. A pitting scale of 0 to 9 should be used to indicate the size and number of
pits on a test coupon. The following ranking should be employed :
Rank
0 No pits. Surface same as for original untreated coupon.
1 Sintered edges (slightly etched edges similar to 200 grade sand paper) but no
pits on major surfaces.
2 Very shallow pits less than pencil point size on edges only.
3 Scattered, very shallow pinpoint pits, less than 25 in number on either surface
(i.e., front and/or back).
4 Very shallow pinpoint pits on either surface to a greater extent than in Rank 3
above. Usually 25-100 over coupon. No major pits as described in 5 below.
5 Ten or less 1/32” to 1/16” diameter. 1/64” to 1/32” deep.
6 11-25 pits of type described in Rank 5 above.
7 More than 25 pits of type described in Rank 5 above.
8 Pits larger than 1/16” but less than 1/8” diameter, 100 or less in number.
9 Any pitting more severe than Rank 8 above.
74
MA-022 Scale Dissolution Capacity Tests (U104/U105/U106)

All tests should be performed in cells pressurized to about 600psi. The scale samples
should be suspended in a basket approximately mid-height in the reactive fluid. The
tests should use technical grade BaSO4 or CaCO3 for comparative purposes.
Test Procedures
• Prepare the scale dissolver (DI water should be used to dilute the chemicals)
• Place 100ml of dissolver into the test cell.
• Weigh approximately 12g of scale sample and place it in a scale basket (no
solubility in scale dissolver), record the weight accurately. (W1)
• Lower the scale basket into the test cell, make sure the scale is located in the
middle of the dissolver fluid.
• Pressurize the cell to 500psi.
• Place the cell in a heating bath for the duration of soaking. (2-24 hours)
• Remove the test cell and release the pressure.
• Filter the contents through a pre-weighed filter paper (filter medium has to be
compatible with filtering fluids) (W2)
• Rinse the solid with water a few times. Place the filter containing solids in a drying
oven.
• Weigh the dried solids and filter paper. (W3)
Scale Dissolution Capacity (%) = (W1-W3+W2)/W1 × 100%
75
MA-023 Acid Response Test Procedure
Introduction
Acid response tests are performed to examine the effect that injected acid has on the
permeability of formation core samples. The permeability before and after acidizing
is obtained to determine the stimulation or damage induced in the core by the
treatment. It is recommended that the treatment fluid volumes be based on
StimCADE simulations, but there are methods of converting the volume injected into
linear cores to a volume required to achieve the same response in a radial flow
geometry.
Temco ARCIII tester (see ARC Tester Operating Procedures for details) or Chandler
Formation Response Tester (See FRT Operation Procedures for Detail)
Cores of either 1.0 inch, 1.5 inches or 2 inches in diameter
vacuum saturation pump
brines, acids and other pumping fluids
Test Procedures
• Measure core dimensions.

• Clean with Toluene until the color is clear if the core is oil-smelly. (no need for
preserved cores)
• Dry the core in oven at 65C for more than 5 hours. (no need for preserved core
plugs)
• Vacuum saturate core in test brine (generally 3% NH4Cl).
• Load the core into the core flow apparatus and apply the confining pressure
(about overburden pressure).
• Flush core plumbing with toluene again at 0.25ml/min until effluent is clear with a
small confining pressure.
• Switch to injection of methanol. Continue flushing the core for 10 pore volumes,
or until the effluent is clear.
• Heat the cell to operating temperature and apply backpressure.
• Measure initial, stable permeability with test brine injected at specified flow rates
at production direction.
• Determine the injection volume and injection rate using the spreadsheet
Required input
---Pump rate in field (bpm)
---Injected volume in field (gal/ft)
---Overflush volume injected in the field (gal/ft)
---Interval height (ft)
76
---Porosity (%)
---Wellbore radius (inches)
---Core length (ft)
---Core diameter (inches)
If the parameters are unknown, then use an agreed upon sequence, such as that
shown as follows.
Mud Acid ARC

• 25 PV 3% NH4Cl Brine at 1.0 ml/min (inject until stable pressure drop is
achieved)
• Inject HCl preflush (10 PV or until stable permeability is achieved)
• Inject Mud Acid (up to 50 PV or until permeability has doubled)
• Overflush with HCl or Brine (3% NH4Cl)
achieved)
• Flow 3% NH4Cl Brine at 1.0 ml/min at production direction again until stable
pressure drop is achieved.
HCl ARC

achieved)
• Inject HCl until wormhole breaks through end of core.
achieved)
• Flow 3% NH4Cl Brine at 1.0 ml/min at production direction again until stable
pressure drop is achieved.
• Shut down pumps and follow Core Flow Apparatus shut-down procedure.
ABOVE PROCEDURES ARE SUBJECTED TO CHANGE REGARDING TO

DIFFERENT TESTING OBJECTIVES AND FLUID SYSTEMS.
77
SECTION 3 FORMATION DAMAGE
FD-001 Immersion Test

Introduction
All cores exhibit different responses to treatment with various fluids. This test offers a
simple method for determining the response of formation cores to a treatment fluid.
Rock hammer
Chisel
Oven
Bottles, 2-4oz
Stopwatch
Treatment fluid
Formation core
Test Procedures
• Break off small pieces of core (about 2-5g) using hammer and chisel. All pieces
are supposed to be the same size.
• Dry the above core pieces in the oven overnight.
• Place each single piece of core in a labeled sample bottle and fill with ¾ full with
the desired fluid.
• Place all bottles in a safe location where they can be observed without moving
them.
• Watch the samples over certain time intervals and estimate the amount of
dissociation that takes place. Record the time and visual observation over an
extended period of time.
78
FD-002 Mud Damage Laboratory Operation (can be adapted to MUDSOLV test)
Introduction
This HTHP operation is mainly for simulating the mud damage on core sample or
collecting sample for static immersion test on mud filter cake.
HTHP filter press (Modified Baroid Cell)
Filter medium
Thermometer
G-Cylinder
High-speed mixer
Mud
Operation Procedures
• Prepare a 1” diameter by 1” length core plug and saturate it in brine solution.
Refer to core preparation/saturation procedures.
• Test initial brine permeability using SCR Formation Damage tester. (modified
Baroid Cell as attached diagram)
• Place the thermometer in the heating jacket and preheat to 10oF above the
desired temperature. Adjust the thermostat to maintain the correct temperature.
• Assemble HTHP cell as required (wrap core sample with teflon and insert to
rubber sleeve, place spring and O-ring for core sample mud damage; place filter
paper for filter-cake collection).
• Stir the mud sample for 10 minutes with the high-speed mixer. Pour the mud
sample into the filter cell, being careful not to fill the cell closer than 30mm from
the top to allow for expansion.
• Complete the assembly of the filter press and with the top and bottom valves
closed, place the cell in the heating jacket. Transfer the thermometer to the filter
press.
• Connect the HP collection cell to the bottom valve and lock in place.
• Connect the regulated pressure source (N2) to the top valve and collection cell,
lock in place.
• With the top and bottom valves closed, apply the pressure of 100psi on both top
and bottom.
• Open the top valve, maintain the 100psi pressure to the mud while heating the
mud to the desired temperature.
79
• When the temperature reaches the desired temperature, increase the top
pressure to 600psi and open the bottom valve for filtration (static filtration
parameters can be determined here).
• After the test period of about 2 hours, close both top and bottom valves on the
pressure cell and bleed off pressure from the regulators. Allow a minimum of 5
minutes for the filtrate to cool to avoid vaporizing.
• Remove the cell from the heating jacket, first making sure that the bottom and top
valves are tightly shut and all pressure is off the regulators. Keep the cell upright
and cool to room temperature before disassembly. Failure to do so could result in
serious injury.
• Place the cell upright and open the top valve to bleed off the pressure from the
cell content until the cell cooled down.
• Open the cell and collect the desired sample (scratch off the top cake on the core
for mud-damaged core sample, wash the filter cake gently on the filter paper for
filter cake collection.)
• Place the damaged the core plug back to SCR formation damage tester and
check the final brine permeability. The mud damage will be reported as
Retained Permeability = Final Permeability/Initial permeability × 100%
Rubber sleeve
Steel locking
ring
Rock core Locking bolt holes
PTFE ring
Core
holder
base
Standard
HPHT
cell base
GAS Regulator
SUPPLY
Pressurised
reservoir for
fluid used in
permeability
calculation Pressure
transducer for
accurate delta P
measurement
Valve stem
Isopar HP/HT cell
mineral oil
Core holder
Rock core sample

Valve stem
Balance logging
8.999 to PC to
measure flow
rate
Schematic Diagram of SCR Mud Formation Damage Tester
80
FD-003 TEMCO ARCIII Tester Laboratory Operating

Introduction
The following is the operation procedure for the ARC machine, to simplify the steps,
each regulator & valve will be given a reference number, please refer to the drawing
plan of the ARC attached.
Reference Valves & regulators label

No. on the drawing plan
1 From pump
2 Return
3 Air/vacuum
4 Core press to core holder
5 Return
6 Vent BPR dome
7 N2 to BPR dome
8 Vacuum to top of accumulators
9 Air to top of accumulators
10 Air pressure to core holder & accumulator
11 Core inlet pressure
12 ∆ P tranducer system
13 Confining pressure
14 Zero 1st ∆ P
15 Zero 2nd ∆ P
16 Zero total ∆ P
17 Core intet to ∆ P
18 1st tap to ∆ P
19 2nd tap to ∆ P
20 Core outlet to ∆ P
21 Core holder heater
22 1st ∆ P
23 2nd ∆ P
24 Total ∆ P
25 Nitrogen to gas flow controller
26 Metering pump
Test Procedures
Preparation
• Need to calibrate and change the diaphragm of pressure transducer according to
N2 permeability. Refer to APPENDIX I.
• On main switch, ARC machine & computer.
• Put core sample into the core holder.
• Set 21 to the desired temperature
81
• Open N2 lines behind ARC machine. Regulate nitrogen inlet for confining
pressure and nitrogen inlet for back pressure.
• As the accumulator was equipped with a piston inside, during pumping, the piston
will move up, hence before any test, the piston need to be push down to make
space for solvent filling, to do so, first close all 1, 2 & 3.
• Only open 1, 2 & 3 required for each one accumulator.
• Open 9 and regulate 10 to 60 psi or higher. This is to push down the piston.
• When required volume reach, decrease regulator 10 to zero, close 9 and close all
1, 2 & 3.
• Do the same sequence from step 8 to 10 for other accumulator.
• Fill solvents into the accumulators/alloy cylinders.
• Close 6, 7, 8, 9, 18 & 19. Open up 14, 15, 16, 17 & 20. NB : 12 & 13 should
always point up to “measure” & “pressurized” respectively.
Confining Pressure
• After temperature reached, close 5 & open 4, pump to desired confining
pressure, increase regulator 11, close 4
• Use Pump Regulator to pump the oil. When pressure reached (the confining
pressure will be indicated on the digital panel, above 23). To maintain the
confining pressure, you can open 4, pump up oil, then close 4 when indicator
indicates confining pressure.
• Wait the temperature and confining pressure until stable before running the test.
ARC Operation
• Make sure the 2000 ml beaker is filled up with water (the pump is linked to it
through a suction tube & the piston inside the accumulator will be pushed up
these water when the pump works).
• Reset 26 by pressing the reset button on it. Set pressure limit by pressing
“high/low” button & turn the knob above them respectively. This step is to ensure
that the flow pressure would not be higher than the confining pressure. (e.g. If
your confining pressure is 600 psi, then set the pump to +/- 59 (*10) psi or
lesser).
Computer
• Check the computer, logo “Temco” & “continue” bar appear on the screen. Use
mouse to click on the “continue” bar, the screen with the flow plan will appear.
82
This screen is mainly use to compare the accuracy of computer data & ARC
machine data. e.g. confining pressure value on the screen & value on the panel,
temperature & etc. If the accuracy is not within 15%, calibration on the computer
may need to perform. (See APPENDIX I).
• Click on “Variable” button, the screen with 6 column should appear. Make sure
that the right hand upper corner shows “Pump/MFM computer control” instead of
“Pump/MFM panel control”. The later is for manual control with the controller on
the ARC machine.
• To begin, first fill up the “Core Data Entry” columns except both “Core length to
first/second pressure tap”. Key in the first fluid you are going to run, cross the
box at the left hand box, click the forward direction, F. Write “Injection Time” as
long as possible, e.g. 50 min. Fill in the Liquid Throttle e.g. 8 cc/min.
• Open valve 1 From Pump which is choosed accumulator.
• When you are ready to run, just click on “Start Process”.
Back Pressure
• After click on the “Start Process” on the computer with the reference fluid, this is
to fill up the line before back pressure is applied. It might take 5 to 6 minutes to
fill up the line. When the line are filled up, effluent will be seen at the exhaust
tubing outlet.
• Slowly open up 7 for the desire back pressure, close it when the “BPR DOME
PRESSURE METER” (found beside 7) shows the back pressure. Excess
pressure can be released by slowly open up 6 & close it again once pressure is
confining P on the meter. If the back pressure is not reaching back pressure
even though 7 is wide opened, it could be that the nitrogen gas is not regulate
enough.
• When back pressure was building up, the fluid will not be seen at the exhaust
tubing, this is because fluid has to flow against the back pressure. When it
overcomes the back pressure, shown on “Core inlet pressure indicator” (above
22), fluid will continue to flow. By this time, test can be run.
83
Running Test
• As the first fluid is still running, what you need to do now is to re-input the
injection time. For example, if 1 pore volume = 3 ml and you want to pump 20
pore volume at 2 cc/min, the injection time should be 3x20/2 = 30 min. Hence,
click on “Reset Process”, click on time value remaining in the “Injection Times”
column. In this case it is the same row as 3% NH4CL. (NB: Do give extra 5
minutes allowance in the input value, ie. input 35 minutes.)
• To begin, click to cross the box at the left hand most, click the forward direction,
F. Fill in the Liquid Throttle e.g. 8 cc/min. When you want to run, just click on
“Start Process”.
• When the fluid flow out to exhaust tubing outlet click on Liquid Throttle box and
change to 2 cc/min or any value you want to run.
• Zero 24 with the left hand side “zero” button, the indicator should show 00.0.
• Close the valve 16, the fluid will then pass through the core & the reading will be
officially recorded. Record the time you start. You may click on the “Trending”
button at the bottom of the screen to see the trend of the flow at specific time,
according to the period you have keyed in (* See APPENDIX III). Go back to
“Variable” by clicking on it.
• After the injection time has ran out, open valve 16 and the ARC will automatically
stop.
• Click on the “Reset Process”, cross the column with 3%NH4CL, put injection time
as 0.1 min. Click “Start Process” with value in “Liquid Throttle” as 0.0 cc/min.
This is to stop the trend line from continue to draw which may cause confusion
when the second fluid is run.
• You can key in the 2nd fluid, e.g. 5% HCL & other data (e.g.. Visc 0.56, injection
time for 10 pore volume 20 min (15 min + 5 min), cross the box B & make sure
the direction is R (Reversed). Key in the flow rate 8 cc/min & click on “Start
Process”.
• Repeat step 29 to step 33.
Finishing
• After the last fluid was flowed, (valve 16 should be opened). You may close the
nitrogen line & open up valve 6.
• Open valve 5, 4 & decrease regulator 11. The confining pressure indicator,
(above 23) should show 0 psi.
84
• Reduce 21 to room temperature & allow the core to cool. (the core cannot be
pulled out if the temperature is still high due to oil expension.)
• Core sample can be taken out after temperature fell less than 90 deg C.
Retrieving Data and Plotting

• Refer to *APPENDIX IV to retrieve the data.
Turn-off Computer
• You may off the computer even if data is not interpreted into graph as they are
stored in the computer.
• To off, press “Alt+Tab” simultaneously and hold “Alt” and keep pressing “Tab” till
Program Manager appear and then release all.
• Click File and Exit window.
• When C:\> appear, turn off the computer.
85
86
87
APPENDIX I
CALIBRATION
1. General information
CORE INLET PRESSURE : Span should be 1884 span
CONFINING PRESSURE : Span should be 1857 span
To do this,
a) Switch ON the ARC machine
b) Adjust zero setting on digital display of CORE INLET PRESSURE and
CONFINING PRESSURE to zero using screw driver. After that, press cal
and adjust span to 1884 (for CORE INLET PRESSURE) and 1857 (for
CONFINING PRESSURE) using screw driver.
For 0.1% accuracy of 3000, allowance is +/- 3
The Panel of
Indicators on the ARC
2. Calibration after changing transducer eg. Disc 40, 12.5 psi.

a) Check the computer, “Temco” & “Continue” bar appear on the screen.
Use mouse to click on “Continue” bar, the screen with the plan will
appear.
b) Goto “Program Manager” (To do this, press “Alt+Tab” simultaneously and
hold “Alt” and give pressing “Tab” till Program Manager appear and then
release all).
c) Click on “Application”.
d) Click on icon of “Window Maker”.
e) A box with few choice will appear, double click on “PROCESS”.
f) A flow plan will appear, double click on the 4th, i.e. the transducer position.
g) You will see a chart under “Value Display” with a ? beside the “Analog”
h) Click on Analog, the words Abs [Pressdrop] will appear, double click on it
(shadow with blue), min & max EU will appear.
i) Key in the value next to EU, to begin, you may type in the psi of tranducer
multiply by 100, e.g. For dish #40 (12.5 psi), type min EU : -1250, max EU
: 1250
For disc #60 (1250 psi), type min EU : -125000, max EU : 125000
88
j) Click on “Done”, “OK”, “Done”, the flow plan will appear.

k) Click File & Save window, the box with “Process” will appear, click “OK”,
the changes woulds be saved.
l) Click File & Exit.
m) Press Alt+Tab to exit the window. After all rebut the computer.
CHECKING
n) To see if the min/max EU value is correct, do a proper test by flow fluid through
the core (after zeroing) & compare how close the 24 value is to the computer
value. If more than 10%, re-input EU value again.
NB : Value in computer divided by 100 = value on ARC, an e.g. as follow
Value on the screen, Value on ARC

psid
0.0 0.002
11.0 -0.0
4.0 0.03
68.0 0.4
89
APPENDIX II
You may use ARC to run Gas Perm which needs 1500 psi of gas.
1) Open N2 line and regulate (for back pressure regulator) to 1500 psi.
2) Regulate 25 to 1500 psi.
3) Make sure 14, 15, 16, 17 & 20 are open, 18, 19 are closed.
4) Zero 24 using the zero button.
5) Similar to step 21, except key the value in “gas” column & fill in Gas Throttle
instead of Liquid Throttles.
NB : a) SLPM stand for Standard Liter Per Minute.

b) The full scale is 3 SLPM (at 1500 psi, the following will show).
Screen, Indication on Gas Mass

SLPM Flowmeter/Liter (below 22)
3 100%
2 67
1 33
0.1 3.3
6) See from step 2 to 40 to run the gas. Fill in Gas Throttle instead of Liquid
Throttle.
90
APPENDIX III
Trending allow you to view to trend of flow test at the specific interval, it is however
not develop currently with the proceed of the flow.
1) The following graph can be seen when click on trending:
To see trend,
click on the
box & see/fill
in the suitable
number
Trending help
2) NB : The chart range min = 0%, max = 100%.

It had been set that 100% = 1000 mD
Hence, each % repersent 10 mD.
3) You can view respective trend using the Tags, to understand what is Perm 11,
Perm 12, Perm 13, Perm 14 and Perm 15.
91
APPENDIX IV
DRAW CHART
1) Click on “Excel File”

2) Click on “Default Setting”
3) Enter each column according to the instruction above the box. To facilitate the
draw of graph, can put requested length of time in between samples as 10S or
20S.
e.g.
Save the
above
range, i.e.
10S
interval
data for 5
hours,
starting
from 13:00
pm, into
file XYZ.
Status :
Error Message :
Send Data/Write to File

Default Setting
Start Msoft Excel
7/26/95 10S
13:00:00
300S C:\INTOUC\HISTORY\XYZ
.CSV
“$DATE, $TIME, PERM11, PERM12,

PERM13,PERM14,PERM15”
PERM 11, PERM 12, PERM 13,PERM14,

PERM15 is the location of fluid (i.e. A, B, C, D
or E). To refer to the ? P across the core,
always be 1 unless we measure the 1st and 2nd
tap ? P.
[click “Trending”, then “Trending help for detail”]
92
4) After everything set, click “Send Data”, if status is “Success”, then click “Writing
to File”, or else “Error” because the data may be too much, to overcome it, can
increase the interval time to 20S or even higher.
5) Click “Start Microsoft Excel”.
6) Microsoft Excel-Book 1 will appear.
7) Click “File” & “Open”.
8) To open the file, go to C:\INTOUCH\HISTORY and choose to ALL FILE.
9) Double click the file name that you save. e.g.“XYZ.CSV”
The following will appear,
$Date $Time PERM11 PERM12 PERM13

7/26/95 13:00:00 200 0 0
7/26/95 13:00:10 203 0 0
7/26/95 13:00:20 298 0 0
11) To draw a graph, you need to edit the above data. First delete all unwanted
figure, cut & paste the valid data from Perm 11, Perm 12, Perm 13, Perm 14,
Perm 15.
12) Next, insert a column next to Perm 11 & type “Pore Volume”.
A B C D
1 $Date $Time Pore Volume Perm
2 7/26/95 13:00:00 0
3 7/26/95 13:00:10
13) Type 0 & enter in C2.
14) Next, click at C3, type formula “=C2+0.1111”, [we use 10 second interval and
assume 2 cc/min, hence every 10S = 0.1111 ml Pore Volume.
13) Copy C3 and paste all the way down the column, the following will show
Vol Perm
0.00 200
0.1111 203
0.2222 198
0.3333 201
0.4444 202
14) To draw chart, highlight both column and click on Chart-Wizard.
15) Bring down the wizard mark to a suitable area and click.
16) Click “Next >”, Click on “Line”, then “Next >”, choose line chart, use 1st column
and 1st row, next.
17) The Chart-Wizard step 5 of 5 will appear, click on “No legend” and fill in the
appropiate data. Finally click as “Finish”.
18) You may modify same point using this chart as a monitor, after all point are
modified, you can draw an exclusive chart.
19) Repeat 14 but click on “Insert”, “Chart”, “As new sheet”.
20) Follow instruction or repeat 16 to 17.
21) Label the chart & draw line as wished.
22) You may save the chart in the disc under different title.
To do so,
1st) go to “File”
2nd) “Save as”
3rd) click ‘a:” and Type Name
23) Fill in the form and put a side one graph for future reference.
93
ARCIII – Temco Acid Response Curve Tester
94
FD-004 Advanced Emulsion Tendency and Demulsification Test
Introduction
Emulsions are always a major concern in acidizing treatments. Downhole, they can
cut production rates. At the surface, they can be very hard to treat. Emulsion
prevention is better than treatment.
Surfactants, mutual solvents and anti sludge agents can prevent emulsions. These
chemicals react differently with various crude oils and formation materials; therefore,
they should be tested before field use. The American Petroleum Institute (API)
developed API RP-42, a standard procedure for testing surface-active agents. The
API procedure does not always accurately model what occurs downhole. Adsorption
near the wellbore can almost completely remove surface-active chemicals from the
acid system. Emulsions may occur because little surfactant, mutual solvent or anti
sludge agent remain in the acid system.
The following tests should be done any time new/different fluid system is pumped or
any fluid is pumped into a new reservoir. Compatibility tests between different
treating fluid also need to be done if pumping more than one type of fluid.
Guidelines for Iron Control and Anti-Sludge/Non-Emulsifier Requirements in Acid
Systems
The objective of this memo is to facilitate uniform acid system test procedures and
acid system recommendations.
Most of our inhibitors and demulsifiers are soluble or dispersible in either oil or water.
Dilute solutions, such as 10 or 20% concentrations by volume, should be made up so
that accurate measurement may be used in these tests. The concentration of
additives should be based on the per cent volume of the treating fluid.
Well fluid should be fresh sample of crude (for oil well including water at the
producing water cut if any) or condensate and water (for gas wells if any). Some
brine can stabilize emulsion.
During the test, well fluid and acid (spent and live) have to be heated up to the test
temperature in separate containers before pouring into a pre-heated measuring
cylinder. The measuring cylinder can be pre-heated in an oven. Once the acid and oil
are mixed and shaken, quickly immerse the measuring cylinder in the water bath
(water level should cover the emulsion level) and record the breakout.
Dowell Acid Systems
1) Control iron:
95
A) Trivalent iron induces precipitation of asphaltene sludge (and elemental

sulfur in sour wells).
B) Divalent iron can precipitate as FeS in sour wells when the fluid pH exceeds
2.
C) Both tri- and divalent iron can form iron hydroxide precipitates when the pH
exceeds ~2 and ~7 respectively.
2) Stabilize asphaltenes and paraffins: Low pH and multivalent metal ions

(particularly Fe[III] ) promote the flocculation of asphaltenes and paraffins in the
form of a sludge.
3) Do not form stable emulsions with produced fluids: Emulsions create high
pressure drops in the near wellbore region and may upset surface equipment.
Dowell uses a combination of acid corrosion inhibitors and iron control agents to
eliminate trivalent iron and prevent iron hydroxide precipitation. Additionally, anti-
sludge and non-emulsifing agents are used in the acid systems to prevent the
deposition of asphaltene/paraffin sludge and prevent the formation of emulsions.
Laboratory tests give a good indication of what anti-sludge and non-emulsifying

agents are required to prevent sludge and emulsions as long as the iron is under
control. Often it is the uncertainty in the expected iron content that complicates acid
system design. The following guidelines are presented as a starting point for acid
system design.
1) Iron enters acid via surface equipment, production or working strings, and the
formation. We can calculate the expected iron content that will enter the acid in
the formation if the mineralogy is known. Additionally, we can control the
amount of iron in the tubing if we can pickle the tubing.
2) Pickle jobs in Sonora, TX: 7000’ of tubing was pickled using three 200 gallon
slugs of HCl. The HCl was pumped down the tubing and then returned to the
surface. The total iron content in the returned acid was less than 2,000 ppm
after the third acid slug on every single well. If your client cannot pickle their
tubing, expect total iron concentrations between 40,000 ppm and 150,000 ppm
during the initial portion of the acid job.
3) Discuss the possible sources of iron with the client and discuss the possible
amount of iron that can enter the acid. Furthermore, make sure they understand
all the adverse reactions the iron can have with the produced fluids and in the
96
formation. Iron control is expensive and clients may not readily understand its
necessity.
4) If you can pickle and verify the iron content is less than 2,000 ppm total iron, it is
safe to treat for a total of 2,000 ppm total iron with a 3:1 ratio of Fe[II] to Fe[III]
(assuming the amount of iron in the formation is know to be small).
5) If you cannot pickle, recommend additives to control 10,000 ppm of total iron
with a 3:1 ratio of Fe[II] to Fe[III] .
6) Iron reducers are the only way to reduce the amount of Fe[III]. Dowell iron
reducers include L63, L58, and XE-72.
7) Chelating agents sequester Fe[II]. Dowell chelating agents include L62, U42,
L1. Acetic acid L400 is not effective (zero activity above 150°F).
8) The best iron control packages will contain iron reducers to eliminate Fe[III] and
chelating agents to prevent the precipitation of ferrous hydroxide and ferrous
sulfide (in sour wells).
9) A good iron control package will reduce the cost of the anti-sludge package
required for sludgy crudes.
Recommende HCl Iron Controlled

d Range
[gpt or ppt]
Temperature
[%]
Range
[°F]
L63 (reducing agent) 75-175 0-20 250 ppm Fe[III]/gpt in live acid
must catalyze with
A179
L58 (reducing agent) 175-400 0-28 50 ppm Fe[III]/ppt in live acid
should catalyze with 200 ppm Fe[III]/ppt at pH ~1
A179
XE-72 (reducing 75-? 0-28 590 ppm Fe[III]/gpt in live acid
agent)
U42 (chelating agent) 75-400 0-28* 38 ppm Fe[III]/gpt
385 ppm total iron/gpt
L62 (chelating agent) 75-400 0-28* 29 ppm Fe[III]/ppt
excess L62 will
precipitate as a
calcium salt
L1 and L400 75-200 0-28 50 ppt L1 and 10 gpt L400
97
combination (chelating controls between 12,000 ppm

agent) Fe[III] to 2,000 ppm Fe[III]
depending on temperature**
50 ppt L1 and 10 gpt
L400 is recommended
* Check Matrix Materials Manual for solubility limits of these additives in different
acid concentrations at different temperatures.
** Check Matrix Materials Manual for amount of iron stabilized at different
temperatures
98
Conversions From ppm Iron to Mass in Grams.
PPM Fresh Water 15% HCl 20% HCl 28% HCl

[grams/liter] [grams/liter] [grams/liter] [grams/liter]
1000 Fe 2+ 2.5919 2.7861 2.8517 2.9605

3+
1000 Fe 4.8401 5.2027 5.3251 5.5284
2000 Total Iron
3 parts Fe 2+ 3.8879 4.1792 4.2776 4.4408
+
1 part Fe3 2.4201 2.6014 2.6626 2.7642
5000 Total Iron
3 parts Fe 2+ 9.7196 10.4479 10.6939 11.1019
1 part Fe3+ 6.0501 6.5034 6.6564 6.9105
10,000 Total
Iron
19.4392 20.8958 21.3878 22.2038
2+
3 parts Fe
12.1003 13.0068 13.3128 13.8210
1 part Fe3+
For Fe2+: grams in table is of FeCl2•H2O (Ferrous Chloride; Mwt = 144.7683
g/mole)
For Fe3+: grams in table is of FeCl3•6H2O (Ferric Chloride; Mwt = 270.298
g/mole)
Wt% Fe2+ in Ferrous Chloride = 38.58%
Wt% Fe3+ in Ferric Chloride = 20.66%
Test Procedures
• API Recommended Practice 42 for both emulsion and sludge tendencies of the
acid with produced fluids. The following modification is done. Treating fluids
should be prepared, as they will be used in the job. All additives at the proper
concentrations and 2000 ppm Fe 3+ should be included. The test will be done
using spent and live acid. Increase iron concentration if necessary depending
upon on surface and wellbore tubular conditions.
• A recommended modification to the sludge test is to filter the bottle contents
through a #41 Whatmann filter (using a vacuum filtration apparatus). Sludge is
defined as precipitates formed when acid & oil are mixed. Mixing acid and oil at
equal volume at temperature is the criteria for API sludge test. The mixture is
poured through a 100 mesh sieve or Whatman #41 filters and the solids left on
the sieve (if any) after washing with warm water & non-plugging oil is referred as
sludge.
99
• Desirable characteristics:
It is desirable for the acid to strip the oil from the glass walls leaving the surface
water wet. Qualitative comments regarding the wettability of the top of the bottle
are recorded:
--- Poor (P) means oil completely wets the upper portion of the bottle and the oil
film is uneven
--- Fair (F) means a very thin oil film coats the top, perhaps with some streaks of
water wet glass
--- Good (G) means the majority of the oil is cleanly stripped off the glass, a very
small number of oil droplets or oil streaks remain
--- Excellent (E) indicates a perfect homogeneous aqueous phase coverage of

the glass
Complete phase separation within 30 minutes at bottom hole temperature,

preferably within 15 minutes.
The volume of acid that has separated from the acid-oil emulsion is recorded at
time intervals. Once the emulsion has achieved its maximum separation,
qualitative observations are made regarding the wettability of the bottom part of
the bottle, the clarity of the acid, and the appearance of the interface. The same
terminology that describes the upper bottle wettability is used to describe the
wettability of the lower portion of the bottle.
Acid clarity after the emulsion has broken is specified as follows:
--- Very turbid acid (VTA, dark cloudy acid, little or no light passes through)
--- Turbid acid (TA, cloudy, light)
--- Slightly turbid acid (STA)
--- Clear acid (CA)
A sharp free flowing interface between the acid and the oil. A comment is also
made indicating the quality of the interface:
--- SFI, sharp flowing interface that has a free sloshing motion when the bottle is
tipped,
--- II, indistinct interface that flows freely when the bottle is tipped.
100
--- RFI, interface does not flow freely and rigid films (usually accompanied by an
emulsion) are present at the interface
--- PI, poor interface with an indistict boundary. Lots of sludge is concentrated at
the interface and the interface does not flow when the bottle is tipped.
The ability of the aqueous phase to strip the oil from the bottle walls upon
inversion of the bottle is recorded as follows:
--- Excellent stripping (ES, oil is immediately and perfectly lifted off the glass)
--- Good stripping (GS, oil is lifted and stripped from the glass, but it may take as
long as 30 seconds to strip the oil and small oil blobs may remain on the glass)
--- Fair stripping (FS, oil films thin and begin to lift off the glass over a couple of
minutes, oil streaks will remain)
--- Poor stripping (PS, aqueous phase does not displace oil)
Absolutely no sludge can be retained on the filter paper
After sitting for at least 4 hours at BHST, the contents of the bottle are filtered
through a Whatman #41 filter. The filter is dried in an oven at 220? F, and the
mass of the sludge retained on the filter is recorded (mass of sludge = mass of
filter with sludge – mass of filter – mass of a blank. The blank is an oven dried
filter used to filter 50 mls of the crude oil sample). This same test can be carried
out at BHST by preheating the oil, acid, and glass bottle prior to mixing and
replacing the bottle with the acid-oil mixture in the temperature bath.
• Tests should be performed with live and spent acid.
• Tests must be performed with new prescription bottles and the bottles should be
discarded after each test. Laboratory glassware that is not disposable and is
used for emulsion tests should be triple rinsed with alternating cycles of deionized
water and 7.5% HCl.
101
Carbonate Acidizing
Equipment/Apparatus
Hamilton beach mixer
100 ml measuring cylinder with stopper
Magnetic stirrer
Syringes
Beakers
Stop watch
Filter papers 10 micron
100 mesh sieve
Formation core, cuttings or CaCO3 chips for carbonate reservoirs
Test Procedures
• Pre mix all additives and 2000 ppm Fe 3+
to the actual treating fluid. The acid
system is studied to detect turbidity, precipitation or separation of any of the
additives. Spend the acid with formation core/cuttings to a pH of at least 4.5. If
formation cuttings are not available, use calcium carbonate chips to simulate
limestone reservoirs or use marble chips to simulate dolomite reservoirs. If dirty
carbonate reservoir is suspected, disperse 2.5 gram of a 80% 100 mesh sand,
10% wt silica flour and 10% wt bentonite mixture. Filter the solution.
• A synthetic spent acid solution comparable to spent 15% HCl may be prepared.
This is equivalent to 15%HCl in which all but the last 1% of the acid has been
spent.
To prepare 1000ml:
920 ml tap water
230g CaCl2, 94-97%
22ml conc. HCl, 37%HCl
3+
Add all additives and 2000 ppm Fe . Slowly add 15-20g of calcium carbonate to
spent the acid. Filter the solution.
• Run emulsion tests with the pre heated produced well fluid and the spent acid
system at 3 ratios
25:75; 50:50; 75:25
• Use 100ml total volume for both phases.
• Add the phase having the smaller volume to the Hamilton beach mixing cup. Add an
equal volume of the larger phase (in the case of the 50:50 mix, start with the oil phase in
the cup)
102
• Begin to mix at 14000 rpm for 15 seconds, slowly add the remaining of the larger
phase, timing the rate so that all the material is in at the end of 45 seconds.
Continue mixing for 15 seconds for a total mixing time of one minute.
• Pour the emulsion into 100ml graduated cylinder. Record the total volume of the
emulsion transferred.
• Start timing the % breakout.
• During the breakout occasional swirling of the cylinder will aid in releasing
emulsion stuck to the glass wall or free droplets of oil or aqueous phase trapped
in the emulsion.
• Repeat all the three tests (25:75, 50:50 and 75:25 = acid :oil ratio) by using live
acid, premixed with all additives and 2000 ppm Fe 3+.
Sandstone Acidizing
This procedure is more similar to downhole conditions and uses more sand than the
RP-42 test. The acid system with additives is drawn through a sand pack rather than
merely being mixed with sand.
1 ea. 9 cm OD Buchner Filter Funnel
1 ea. 9 cm OD Whatman No. 4 Filter Paper
1 ea. Sidearm Flask
Pack Material: Formation core material or Mixture of 10 wt. % Illite bentonite + 10 wt.
% Silica Flour + 80 wt. % 100 mesh sand
Solution of 3% NH4Cl
Several 100 ml Graduated cylinders
Vacuum pump
Blender and jars
Rheostat
Test Procedures
• Mix 100 ml of the acid system to be tested. The acid system should contain the
recommended concentrations of all chemicals i.e. corrosion inhibitor, iron control
agent, mutual solvent, surfactants, acetic acid etc. 2000 ppm ferric chloride is
added to evaluate the sludging tendencies. The acid system is studied to detect
turbidity, precipitation or separation of any of the additives.
• Prepare a filter pack by placing approximately 200 cc (1”) of the blended pack
material or formation core material into the Buchner funnel containing one No. 4
Whatman filter. Wet the filter paper before adding the pack material.
103
• Water wet the sand pack with 50 ml 3% NH4Cl. Be careful not to saturate the
pack with NH4Cl in order to minimize dilution effects.
• Place Buchner filter funnel into sidearm flask, apply vacuum and filter acid
system.
• If the above cannot be done; pour the acid into the pack material in the Cell of the
API Filter Press (Baroid Testing Equipment) and apply 40 to 80 psi into the cell
with CO2 gas bottle. The last choice would be to spent the acid with excess
crushed pack material.
• Collect 50 ml of filtered acid into a clean graduated cylinder. Add in 50 ml of oil
which has been pre heated to the bottomhole temperature of the well. Test to be
repeated for 25:75 and 75:25 ratio.
• Blend the oil and acid mixture for approximately 30 seconds under high shear
conditions.
• Pour the mixture back into the 100 ml cylinder and place into a hot water bath set
at the bottomhole temperature of the well.
• Measure volume % acid drop out at 5 minutes intervals. This procedure considers
a 90% breakout in 10 minutes and essentially 100% breakout in 30 minutes as
satisfactory compatibility. In addition, the overall fluid quality should be observed
(oil quality, water quality, presence and rigidity of interfacial layer, wettability and
sludge sensitivity).
• All the above to be repeated with live acid.
Demulsification Tests
These tests should be run in the same manner as the emulsion tendency tests. The
Oil-Acid ratio should be that which was slowest to break out in the compatibility tests.
It is usually best to test all demulsifiers at the same concentration for comparative
purposes. The best demulsifiers should then be run at various concentrations in
order to determine the optimum amount.
104
FD-005 ClearFRAC Emulsion and Break Test

Introduction
The high content of paraffin and asphaltene in the produced crude are commonly
associated with emulsion problem of ClearFRAC and crude oil. The emulsions
formed will inhibit the cleanup of the formation and proppant pack. Following
procedures will describe how to identify the emulsion problem using ClearFRAC and
how to break it properly to recommend a proper treatment in the ClearFRAC field
operations.
Emulsion Procedures
• Preheat the clearfrac fluid and crude oil in water bath to desired temperature.
• Mix 50ml/50ml of ClearFRAC/crude oil in an API test bottle, cap it and shake
vigorously for 30 seconds.
• Place the bottle in preheated water bath and start the stopwatch.
• Record the volume of bottom layer and volume of the emulsion at 1, 5, 10, 15,
30, 45 and 60 minutes.
• Calculate the percentage of emulsion break using following equation.
% emulsion break = volume of bottom layer/volume of clearfrac fluid × 100%

Apply breaking procedures below if not greater than 90% emulsion break in 60
minutes.
Break Procedures
• Following fluids are generally used to break (treat) the emulsion problem on
clearfrac.
Fluid I--- 90% water/10% U066 in volume percentage
Fluid II---73-92vol% 2%KCl/5-15vol%/3-12vol% J530
• Preheat treatment fluid, clearfrac and crude oil in waterbath.
• Mix the fluid mixture of crude/treatment fluid as follows and shake for ten seconds
---45ml/5ml; 40ml/10ml; 35ml/15ml; 30ml/20ml.
• Mix above mixture with 50ml clearfrac to shake hard for 30 seconds.
• Place the final mixtures into the preheated waterbath and watch for emulsion
break as follows.
• Calculate the percentage of the emulsion break.
% emulsion break = volume of bottom/(volume of clearfrac + volume of treatment
fluid) × 100%
105
FD-006 Fluid Loss Testing (Microfracture simulation)

Introduction
The test modifies the traditional fluid loss testing with a change in the tested core
plugs to simulate the fluid loss behavior inside a formation containing natural
fractures. This method is useful to evaluate how effective is the fluid loss agent or
diverting agent on the bridging of the natural fractures which is mainly contributing
the high fluid loss property. All operating procedures (safety and equipment list) and
parameters (spurt loss and loss coefficient) determination is the same as those
described in method 03-002.
Procedures
• Select two core plugs (1” by 1”) with permeability of less than 0.1mD.
• Using the core cut-off saw to cut the core along the length, making sure that one
half is little bit greater than ½” thick. Discard the half with less than ½” thickness.
• Sand and file the core plug until the same length and diameter obtained as the
original core plug after placing them together.
• The size of the microfracture can be controlled by the grit of the sand paper used
to sand off the face of the fracture. If high permeability fracture is needed, a small
piece of brass shim stock can be cut and placed between the two core halfs.
• Mount the simulated fracture core plug into the modified Baroid cell (same as
MUDSOLV tester) and run the same fluid loss (filtering) testing to check the fluid
loss behavior of the fluid on the microfractured core plug.
• This test is just used for comparison of fluid loss control effectiveness of different
fluid loss control agents. The physical significance of each individual test result is
not determined.
106
FD-007 Procedures for Compatibility of Formation Brine and Completion Brine

Introduction
Following procedure describe a semi-quantitative evaluation of the compatibility
between the completion brines and formation (reservoir) brine (fluid). The pre-
filtration of the initial brine is simulating the filtration procedures for the field operation
on completion brine injection. Thus the filter paper used in the test can be changed
accordingly to be close to the filter medium used in the field.
Filter unit (crucible/pump, paper)
Analytical balance
Water bath and dry oven
API mixing bottles and other lab glassware
Tested brines
Procedures
(1) Prepare completion brine and formation synthetic water as requested (prefer to
have the original completion brine and formation water with no need to pre-filter)
and filter them through #41 whatman (change accordingly if different filter
medium used in the field). The filtrate will be used for compatibility tests.
(2) Pre-weigh the #41 Whatman filter paper (W1), filter 50ml of completion brine with
addition of 200ppm iron through #41 Whatman.
(3) Dry the residue and filter paper in the oven at 100C and re-weigh the filter paper
+ residue recorded as W2.
(4) Repeat step (2) and (3) for 50ml formation brine (recorded as W3 and W4 for pre-
weigh and re-weigh)
(5) Calculate the residue from individual fluid (completion with iron contamination and
reservoir brine) as follows
A = W2 – W1 B = W4 – W3
(6) Mix 50ml synthetic formation water and 50ml completion brine with 200 ppm iron.
All mixing is under room temperature and atmospheric.
(7) Filter the mixture through #41 whatman again to measure the residue content (C).
(8) Calculate the incompatibility residue of different fluid mixtures in g/100ml mixture.
X (g/100ml mixture) = C (g/100ml mixture) – A (g/50ml CB) – B (g/50ml FB)
107
FD-008 Critical Velocity Determination for Fines Migration Study

Introduction
Fines can be variety of materials presented in the formation rock including clays and
silts. The mechanical movement carried by the fluid flowing across the formation rock
cause the fine particles plug the pore throats in the rock and reduce the rock
permeability in the near-wellbore region. Critical velocity is refer to the maximum flowing
velocity of the fluid through the formation core above which a significant permeability
drop (10-20% above) will happen due to the plugging of the pore throats by the moving
fines. Following is a typical core flow testing procedure to determine this important
parameter using Formation Response Tester from Chandler Engineering.
Formation Response Tester or ACR III
Core preparation/cleaning apparatus
Core saturation apparatus
Core plugs
Brines, Toluene, Methanol
Procedures
(1) Prepare/clean the core plug as described in method 02-023. (flow toluene/methanol
through the core until clear effluent before flowing brine in step (3))
(2) Vacuum saturate the core plug with 10% KCl (generally enough to inhibit the
reactive/dispersive clays) for more than 15 hours. Measure the core size before
furthering tests.
(3) Flow the above brine solution in production direction at 0.25cc/min with 1000psi
confining/500psi back pressure until a stable permeability obtained.
(4) Increase the flow rate to 0.5cc/min to repeat the above test.
(5) Drop the flow rate to 0.25cc/min after step (4) to the stable permeability.
(6) Keep increasing the flow rate and repeat step (5) until observing the permeability
drop of 10-20% (based on 0.25cc/min permeability in each stage).
(7) The flow rate mentioned in step (6) will be recorded to determine the critical velocity
by
(8) Correlate the above parameter to well flowing rate based on provided well
configurations (flowing fluid PVT, wellbore diameter, interval height).
Critical Velocity = Critical flow Rate Recorded / Cross-sectional Area of Tested Core
108
FD-009 Determination of Critical Brine Concentration for Swelling Clay
Introduction
Some clays such as smectite or smectite/illite mixed layers are swelling (volume
increasing more than 6-10 times) if salinity of the flowing brine is not enough to inhibit
this swelling behavior. Depend on the content, chemical nature and location of these
clays in the rock, the degree of the swelling is different. Following testing is designed to
evaluate the clay swelling behavior in the lab.
Formation Response Tester or ACR III
Brines, Toluene, Methanol
Core plugs
Procedures
(2) Vacuum saturate the core plug with 10% KCl (generally enough to inhibit the
reactive/dispersive clays) for more than 15 hours.
(3) Flow the above brine solution in production direction at determined critical velocity
(see method 03-008) with 1000psi confining/500psi back pressure until a stable
permeability obtained.
(4) Drop brine concentration to 8%, 6%, 4%, 2% and DI water to repeat step (3) until a
10%-20% permeability decreasing observed, which is recorded as critical brine
concentration to inhibit reactive clays.
109
FD-010 Dynamic Leak-off and Retain Permeability Testing

Introduction
The leak-off rate of fracturing fluid into the formation during the hydraulic fracturing
operations is one of the most important issues involved in the determination of fracture
geometry for a given treatment design. Two methods of evaluating the fluid loss
behavior of fracturing fluid in the laboratory in addition to the post-fracturing analysis
from the field job evaluation, they are static and dynamic fluid loss testings.
Static fluid loss behavior measured from static (API RP39) fluid loss testing (modified
Baroid cell in method 03-002) are generally underestimating the actual leak-off of
fracturing fluid flowing across the fracture face due to the static testing conditions.
Following procedures describe in detail the method of testing dynamic leak-off
parameters of fracturing fluid and the formation damage caused by the fracturing fluid
after the leak-off testing.
Formation Response Tester
Brines, Toluene, Methanol and fracturing fluid
Core plugs
Procedures
(2) Vacuum saturate the core plug with brine (concentration determined in 03-009)
for more than 15 hours.
(3) Record core dimensions and clean
(4) Load the core into the core flow apparatus and apply the confining pressure
(1000 psi optional).
(5) Heat the cell to operating temperature and apply back pressure (100 psi
optional).
(6) Measure initial, stable permeability with test brine injected in the forward direction
(production direction) at critical velocity determined in 03-008.
(7) Perform dynamic leakoff by injecting the fracturing fluid in the reverse direction
(treatment direction for 64 minutes with pumping pressure 500psi and flow rate of
1000ml/min (which gives us shear rate of 60 sec-1), observe and record the
filtrate volume with time duration (1, 4, 9, 16, 25, 36, 49, 64 81, 100 minutes).
110
(8) Measure final stable permeability with test brine again injected in the forward
direction at same mL/min in step (6). Calculate regained permeability.
Chandler 6100 Formation Response Tester
111
SECTION 4 CORE ANALYSIS

CA-001 Core Porosity Determination
Introduction
Porosity is defined as a ratio of the void-space volume to the bulk volume of the
material.
Measurement of bulk volume (BV) and grain volume (GV) yields pore volume (PV) by
difference and porosity (ø) by:
PV = BV – GV
Ø = PV/BV = (BV – GV)/BV
The bulk volume is determined by Mercury Immersion Method and the grain volume
is measured by Boyle’s Law Double-cell Method. The porosimeter should be
calibrated for V1 and V2 determination. This calibration is required whenever we are
changing the connections shown in the picture.
Bulk Volume Determination --- Mercury Immersion Method
See picture attached for apparatus detailed.
Mercury
Core sample
Test Procedures
• Switch on the apparatus.
• Zero the scale by turning the screw on the scale until pointer touches mercury
colume in the LHS mercury cylinder. (the light just comes on).
• Carefully place the core sample with a wire hook in the RHS mercury cylinder.
• Completely immerse the core sample, eliminating all air bubbles/pockets.
• Turn screw on scale until the light is just extinguished.
• Record the reading.
• Repeat the above test 2-3 times and take the average.
• Actual bulk volume (BV) is obtained from the pycnometer reading – volume
conversion table.
• Power off the apparatus. Keep it safely.
Grain Volume Determination --- Boyle’s Law Double-cell Method
See picture attached for detailed instrument
Nitrogen
Core sample
112
Test Procedures
• Start with all valves closed (open in the vertical position), supply N2 to the line a
little above 200psi.
• Leave valves B (test valve) and C (bleedoff valve) closed and open valve A (P1
LOCK-IN), pressure up to 200psi with regulator.
• Load the sample to be measured into the researvoir and tighten down until the
seats are in line as indicated on the researvior.
• With valve A (P1 LOCK-IN) open pressure up to 200psi (preferably for 0.1psi
accuracy). Close valve A allowing P1 to stabilize. Record P1.
• With valve C (bleedoff) closed, open valve B (P2 TEST VALVE) allowing N2 to
expand into the loaded test reservoir. Record P2 if the reading is stable. Vlave A
(PI LOCK-IN) is closed at this time)
• Open valve C (bleedoff valve) to relieve the pressure for second test.
• Decrease the regulator all way to off.
• Open valve A (P1 LOCK-IN) and close valve B (P2 TEST VALVE) and valve C
(bleedoff valve). Repeat the above procedure for the second test on the same
core sample.
Calculation
V1, system volume to valve B
V2, entire empty system volume
Vr, reservoir volume
GV, core grain volume
BV, bulk volume
Ø, porosity
V3 = [V1 + (Vr – GV)]
P1V1 = P2V3
V3 = P1V1/P2
GV = V2 – V3 = V2 – P1V1/P2
Ø = (BV – GV) / BV
113
Bulk Volume vs. Pycnometer Reading
18.500
16.500 y = 0.9763x + 5E-13
Bulk Volume
R2 = 1
14.500
12.500
10.500
8.500
6.500
7.00 9.00 11.00 13.00 15.00 17.00 19.00
pycnometer reading
Mercury Pycnometer – Bulk Volume Determination
N2 Porosimeter – Porosity Determination
114
CA-002 Gas Permeability Determination

Introduction
Dowell air permeameter is designed to measure the permeability to N2 gas of a
clean, dry, 1× 1 inch core plug. Measuring the differential pressure and flow rate
as N2 passes through the core. Darcy’s equation is used to calculate permeability.
See the attached figure for the instrument.
Core plug
Test Procedures
• Place a dry 1×1 inch core into the rubber core holder (No. 1) shown in the figure.
• Place the rubber core holder into the stainless steel sleeve.
• Load the stainless steel sleeve and rubber core holder into the core holder
assembly of the permeameter. Secure core holder assembly (No.3) using handle
located on the bottom of the assembly.
• With three flowmeter valves (No.4) closed and regulator backed off, supply the
main N2 source to the permeameter.
• Slowly open the flowmeter valve (large) and slightly tap the flowmeter if the ball
inside the flowmeter is rising too much.
• Slowly increase the N2 driving pressure to 0.25 atm by using the regulator (No.5).
• If the reading is below 20 division (0-150 division on the flowmeter), close large
flowmeter valve and open the medium one. The driving pressure is also slowly
adjusted to 0.5atm. Close it and open the small flowmeter valve with the
adjustment pressure of 1atm if the reading is still below 20 reading division.
• Repeat the above step and take the reading until the proper pressure and
flowmeter valve is determined. The reading should be taken to the nearest
division with estimation of the center of the floating ball in the flowmeter.
Calculation
The permeability of the core sample being tested is calculated by Darcy’s equation
K = (µ × Q × L) / (A × P)
Where:
K, permeability in darcys of the sample. (multiply by 1000 to obtain milidarcys)
µ, Viscosity in cp of the N2 gas for making the measurement at the observed
temperature. (taken from the attached viscosity-temperature curve)
Q, Average flow rate in cc/second in the sample at mean pressure derived from the
flowmeter reading and the calibration curve of the flowmeter.
115
L, length of the sample in cm

A, Crossectional area of sample in square centimeters
P, pressure gradient in atm, indicated by pressure gauge
N2 Permeameter – gas permeability test
116
CA-003 Rock Mechanics Test (dry core triaxial compression)

Introduction
ELE triaxial mechanics tester and a TDS-301 data loggger are used in our lab for the
determination of basic rock mechanics properties such as Yong’s modulus (E),
Poisson’s ratio (ν) and Failure compressive strength (σmin).
ELE Triaxial Mechanics Tester with control panel and loading frame
Test cell
TDS-301 Data Logger
Strain gauge with appropriate connections to core sample, test cell and data logger
Core sample being tested (3cm × 6.5cm)
multimeter
Test Procedures
Sample preparation
• Drill a 3cm diameter core plug along the direction of perpendicular to the
overburden stress.
• Cut the plug to 6.5cm in length.
• Polish both ends with polishing machine. The time for polishing one side is 0.5hr
at 20-30 rpm.
• Dry the core plug in oven at 50oC.
• Measure the diameter and length. Sides of the plug should be straight to within
0.05 cm. End surfaces shall be lapped to a torlerance not to exceed 0.003cm.
Gauge sticking
• Make sure the surface of the plug is smooth, polish with fine sandpaper or paint
with some glue and then polish with sand paper if the body surface is not smooth.
• Place the strain gauge and the connector on a glass slide, stick a piece of
transparent tape on the slide and slightly tear off so that the gauge and connector
will be stuck to the tape.
• Stick the transparent tape with gauge and connector on the core as following
diagram. Make sure the gauge is at center.
• Tear half of the tape off to see the back of the gauge. Apply a layer of super glue
on the back of the gauge and connector and stick back to the plug body with
gently rubbing. Tear the tape off and place a new tape strip to protect the gauge
(axial gauge).
117
• Repeat the above steps to place another gauge in the horizontal direction as
shown in the following diagram (radial gauge).
• Cut three pieces of 16cm blace wire and red wires respectively. Solder the wires
as indicated below and check the continuity with multimeter. (120Ω and 0Ω
should be shown)
• Wrap the wire with small piece of tape on the top of the core to prevent cut-off of
the wire by confining pressure during the test.
TDS-301 programming
• Turn TDS-301 data logger on.
• Set key to “free”.
• Press “prog” [program 0-CH]
• Press “0” [F***L***M***]
• Change to [F000 L002 M000] by using “→” key. [F000 L002 M000]
• Press “Entry” [Program 1-coefficient]
• Press “1” [C***-*** 1.000]
• Change to [C000-000 1.000] by using “→” key. [C000-000 1.000]
• Press “ * ” [C001-002 1.000]
• Change to [C001-002 0.943] by using “→” key. [C001-002 0.943]
• Press “Entry” [program 2-point]
• Press “ 2 ” [point *** - *** *]
• Change to [point 000-000 3] by using “→” key. [point 000-000 3]
• Press “ * ” [point *** - *** *]
• Change to [point 001-002 6] by using “→” key. [point 001-002 6]
• Press “entry” [program 3-unit]
• Press “ 3” [U***-*** **=u]
• Change to [U000-000 17=mv] by using “→” key [U000-000 17=mv]
• Press “ * ” [U***-*** **=U]
• Change to [U001-002 00=u] by using “→” key [U001-002 00=u]
• Press “ entry ” [program 4-time]
• Press “ 4 ” [** ** ** **:**]
• Change to default time by using “→” key [Y M D HR:MIN]
• Press “entry” [5 interval]
• Press “ 5 ” [00: 00:10 N00 S01]
• Press “entry ” twice and set key to “LOCK”
Bleed off air bubbles
118
• Turn confining pressure wheel to 10 rounds.

• Open cap of test cell.
• Push bleed valve into the bleed tube, screww and tighten bleed valve.
• Switch on CPU switch and close CPU dump valve.
• Hold bleed valve vertical until oil flow out with an oil pan bottom to collect the oil.
• Pull out valve, trun off CPU switch and off CPU dump valve.
• Clean up bleed off valve and cap. Recap the bleed tube on the test cell.
Loading sample
• Insert sample wwith gauge into the test cell with shorter SS fitting on the top and
longer SS sample extender on the bottom. Solder sample wires to connector on
the top of test cell accordingly. (axial to axial, radial to radial, black to black and
red to red wire)
• Check the continuity of the connection with multimeter.
• Switch on CPU and off the CPU dump valve, holding the SS bars on both sides of
the test cell. All sample and SS bars should be confined into the test cell. Make
sure there is no air bubble trapped in the rubber sleeve inside the test cell (refer
to air bubble bleed off procedure to bleed them off if some).
• Switch on VSPP.
• Place the test cell containing sample and wire connection on the loading fram.
Close VSPP loading release valve.
• Adjust ‘VSPP knob’ and ‘rate increase’ (increase to go faster and decrease to
slow down) until ‘LOAD KN’ on the control panel indicates 1-3KN.
• Reduce ‘VSPP knob’ BACK TO 10-20 and ‘rate increase’ back to zero.
Applying confining pressure
• Go to ‘pace mode’ on control panel, switch from ‘pace zero’ to ‘pace’ and ‘reset’
and then come back to ‘pace’. Adjust the second digit and first digit of the
‘increase pace rate’ until the needle is at the center of the ‘loading pacing error’
indicator. Switch from ‘pace’ immediately back to ‘pace zero’. Set the ‘increase
pace rate’ to ‘0-0-4’.
• Turn ‘pace zero’ back to ‘pace’ and start applying confining pressure. Make sure
the needle should always be kept at the center of the ‘loading pacing error’
indicator while you apply the confining pressure by adjusting both loading wheel
and ‘rate increase knob’.
• Stop loading when the black needle reaches the red needle (confining pressure
requested).
• Repeat the ‘pace mode’ setting procedure and reset the ‘pace zero’.
119
Start testing
• Switch ‘pace zero’ back to ‘pace’.
• Initialize the gauge and check the continuity by set key ‘free’ and press ‘Init’ and
‘start’ simultaneously. Set key back to ‘Lock’ and then press ‘start’. The continuity
is ok if data around 00000.00 shown on the printout slip.
• Set the ‘Interval’ on and press ‘start’ to initialize the test.
• Inrease the load at set pace for 10-30 KN more (10KN for soft core and 30KN for
hard core) to test the core mechanical properties. Always keep in mind that the
needle should be at the center of the ‘loading pacing error’ indicator while
applying loading by adjusting the ‘rate increase knob’.
After testing
• Turn off ‘Interval’ of programmer.
• Release load slowly until we get back to original load (of about -20KN of max) of
confining pressure.
• Repeat two more tests.
• Check the test results and calculate Yong’s modulus and Poisson’s ratio.
• If the results is OK, keep concentrate on the loading indicator while continuously
increase loading until the core fails. (A big sound should be heard at this
moment). Record the failure loading (prefer to using TDS-301 to record the data).
• At the end of test, release load and confining pressure at the same time slowly.
Do not overturn any one of them (as a rule of thumb, keep load reading about
70% of confining pressure.)
• Hold test cell and release ‘VSPP release valve’ and switch off the VSPP.
• Release CUP dump valve and turn it off. Take the SS bars out of the cell.
• Desolder the core wire and turn off TDS-301.
Calculation
The following equations are used for calculating Yong’s modulus and poisson’s ratio.
EV = L / (A × SV)
EH = L / (A × SH)
ν = EV /EH
120
Where,
EV: axial Yong’s modulus, psi
EH: horizontal Yong’s modulus, psi
SV: axial strain, ×10-5 (from TDS-301)
SH: horizontal strain, ×10-5 (from TDS-301)
L: load, Kn(from TDS-301)
A: cross-sectional area of core plug, 0.693 ×10-3 m2
ν: poison’s ratio
Plot the straight line with Stess-Strain data sheet (linear regression) from above
equation in the Excel spreadsheet, the slope of the line is Yong’s modulus and the
ratio of axial and radial Yong’s modulus is Poisson’s ratio.
A sample calculation is attached for reference.
reading Load Load Axial Strain Radial Strain

mV kN Mpa 1.00E-05 1.00E-05
20.684 94 119.5
21.93 1.246 1.79798 3.6 0.4
23.766 3.082 4.44733 12.5 0.8
24.589 3.905 5.634921 16.3 1
25.934 5.25 7.575758 22.1 1.2
26.652 5.968 8.611833 25.7 1.3
27.784 7.1 10.24531 30.3 1.5
28.88 8.196 11.82684 35.9 1.9
30.039 9.355 13.49928 40.5 2.1
31.288 10.604 15.30159 46.6 2.5
32.076 11.392 16.43867 49.9 2.8
33.221 12.537 18.09091 54.8 3.1
34.459 13.775 19.87734 60.2 3.3
35.735 15.051 21.71861 65.3 3.5
36.428 15.744 22.71861 68.1 3.8
37.486 16.802 24.24531 71.8 4.1
121
Strain vs. Load

80
y = 3.0547x - 0.903
70
60
Strain (10E-5)
50
40
30
20
y = 0.1664x - 0.0209
10
0
0 10 20 30
Load (MPa)
ELE Triaxial Rock Mechanics Tester
122
CA-004 SEM/EDAX Sample Preparation for Petrographic Core Analysis

Introduction
Although wet mode is available on ESEM instrument in our lab, it is recommended to
use coating mode (vacuum) to run core petrographic analysis by ESEM/EDAX
combinational analysis. Generally three main steps regarding to a proper sample
preparation of core sample for ESEM/EDAX vacuum mode analysis. They are pre-
cleaning, sample sticking and sample coating. Following procedures describe in
detail.
Gold-coating or graphite-coating machine
Toluene/CCl4 and methanol
Conductive glue (silver paste)
Sample platform (Aluminium)
ATTENTION BE PAID ON VERY POISONOUS CCl4 WHEN USED!!
Procedures
(9) Modify (file/sand/chisel) a small piece of sample (core fragment or cut from core
sample) to a parallel bottom and top surface without touching the top surface.
(10) Clean with solvent (toluene and methanol, CCl4 needed if very heavy oil
presented in the core sample)
(11) Dry the sample in the oven at 65C. Being cautious on the top surface (do not
disturb).
(12) If sample surface was observed to be dusty/contamination, a ultrasonic
cleaning will be necessary by acetone and then repeat the drying step (3).
(13) Use double-face tape or silver glue to stick the sample on the sample
platform. Be reminded to create a glue/paste bridge between the sample and the
sample platform, which is very critical to neutralize the charging in the microscope
analysis.
(14) Dry the whole sample sticking on the platform in the oven again at 65C for an
hour.
(15) Open Argon Gas Valve and Adjust Regulator to 10 psi.
(16) Place the sample into the Chamber.
(17) Before the starting, make sure ARGON LEAK VALVE is in ‘clock wise’
position and kV is ‘anti-clock wise’ position.
(18) On the pump.
(19) When the torr reach to 0.2, Open ARGON LEAK VALVE ‘anti-clock wise’ to
purge the air.
123
(20) After that Close ‘clock wise’ direction ARGON LEAK VALVE.
(21) Repeat step 5 and 6 when torr reach to 0.1.
(22) Repeat step 5, 6, 7 for 2 - 3 times.
(23) When torr reach to 0.06 is ready to start coating.
(24) Turn knob to SET HT.
(25) Turn kV ‘clock wise’ to 2.5 or 2.6.
(26) Adjust ARGON LEAK VALVE ‘anti-clock wise’ slowly until kV reach 18 or 20
mA.
(27) Set HT to MODE position.
(28) Press timer (it is about 3.5 minutes setting).
(29) After timer reach zero and ampere goes to ‘0’, then the coating is finished.
(30) Turn kV ‘anti-clock wise’ all the way just to the end (do not over turn).
(31) Turn ARGON LEAK VALVE ‘clock wise’ all the way just to the end (do not
over turn).
(32) Turn the knob to OFF position.
(33) Close Argon Gas valve and adjust Regulator to Decrease position.
(34) Bleed off the vacuum chamber slowly.
POLARON SEM Gold-Coating Unit E5100
124
CA-005 Bulk XRD Sample Preparation Procedures

Introduction
Powder sample packed on a plastic sample holder is generally used for XRD powder
diffraction analysis on bulk mineralogical information. Two aspects are generally
important in preparing powderous XRD bulk analysis samples. They are random
particle orientation and packed flat powder sample surface instead of loose, cracking
or disintegrated pack. Following procedures list the detail information on how to
properly prepare a packed powder sample for XRD powder diffraction analysis.
Grinding ball mill with auto control on timing and rotating speed
Sieves and Mortor
Sample holder
Glass plate
Methanol/chloroform
Procedures
• Roughly grind the core fragment with mortor to less than 1mm particles.
• Clean with chloroform/methanol if sample is not clean, dry it in the oven at 65C
for more than 3 hours.
• Place the powder into a ball mill with one alloy ball inside. Install it on the ball mill
machine to grind the sample. (generally 65 amplitude for 3 minutes is enough to
get a particle size of less than 10-20um)
• Carefully place enough powder sample on the groove of the plastic sample
holder. Gently pack the powder to the groove (rotate the glass plate at 90 degree
angle) using a glass plate until a random orientated, tight packed powder pack in
the holder groove.
• Gently get rid of the extra powder resides on the edge of the holder groove.
• Pack the powder on the top surface using a glass plate to make a flat top surface,
continue above packing until that the sample will not be easily slided away if we
tilt the whole sample at 80 degree angle.
RETSCH MM2000 Grinding Mill
125
CA-006 Total Clay Content Determination
Introduction
This method, which is based on Stokes Law, is applicable for determination of total
clay content in sandstone/carbonate and claystone. The analysis is testing the clay
particles less than 5um in sandstone or carbonate and less than 2um in claystone.
Analytical balance
Centrifuge and accessories
Ultrasonic Suspender/Dryer
Mortar/Glass rod /300ml beaker
DI water/Toluene/15% HCl
Clay flocculating agent (L055)
Procedures
(1) Grind samples to less than 0.5mm
(2) Clean with toluene if sample containing oil until colorless.
(3) Measure powder sample of about 5 grams accurately by analytical balance.
Record as W 0
(4) Place the sample in the 300ml beaker and add DI water 250ml, stir with glass
rod.
(5) Place the beaker with mixture in ultrasonic machine for further suspending.
(6) If not suspending, check the bulk XRD scanning see if carbonate or inorganic salt
presented.
(7) Decant the water and add 15% HCl to react until no bubble observed if carbonate
presented in bulk XRD. Clean the reacted residue with DI water until the clay start
suspension.
(8) If inorganic salt presented, use DI water to wash the sample until sample start
suspending clay.
(9) Pipette the clay suspension carefully (tip at 2cm above the solid precipitates at
the beaker bottom) to another 300ml beaker, add 0.5ml of flocculating agent and
wait for 24 hours flocculation.
(10) Decant the clear part in the beaker and wash the flocculated clay into the as-
weighed centrifuge tubes (record as W 1).
(11) Centrifuge the tube with clay suspension at 3000rpm until transparent liquid
on the top.
(12) Decant the water and Place the tubes with wet clay into the dryer at 65oC.
(13) Re-weigh the tubes with dried clay (record as W 2) to calculate the clay weight.
126
(14) Repeat above steps from (4) to (13) on the precipitates in the first beaker until no clay suspended.
Calculation
Total clay content is calculated as X = (W2 – W1) / W0 × 100%
127
SECTION 5 SAND CONTROL AND WATER CONTROL

SC-001 Semi-quantitative PSD Analysis by SEM Imaging
Introduction
PSD data of the formation sand is very important for well completion program
especially the gravel and screen selection. API sieve analysis (if enough sample
available), Thin-section/imaging analysis, Laser-diffraction unit analysis are generally
the methods used to obtain the PSD information on the formation sand. The
methodology described in this procedure is similar to thin-section/imaging analysis
but with less accuracy as no imaging analysis software is applied in the imaging
system.
ESEM
Gold-coating system
Formation sand sample
Procedures
• Refer to the procedures on preparation of an ESEM gold-coating sample.
(method 04-004)
• Pick up nine spots on the round shape sample image as indicated below and
take the proper (spot size, magnitude, contrast, brightness) SEM images.
• Using the ruler tool in SEM measuring function to measure the long dimensions
of 100 typical grains in each image picture and record. (record the long
dimensions of the pores for pore size distribution analysis)
• Group the size of the grains in 25-50um interval depending on the results
recorded and locate all data recorded above into these groups.
• Calculate the number percentage of each group grains among the whole grain
numbers we collected in the images and then derive the “s” plot for pore size
distribution or grain (particle) size distribution. Based on number percentage
instead of weight percentage.
128
SC-002 Gravel and Screen Selection from PSD Information of Formation Sand
Introduction
Gravel packing is depend on how we properly bridge the formation sand grains in the
larger particles of gravel, which itself will be retained by a screen or slotted liner.
Thus, the PSD information from the formation grains and the methodology used to
size the gravel and screen is very important in gravel pack completions. Following
methods are used in our lab to size and select the gravel and screen based on PSD
data tested in the lab (either sieve analysis, SEM image analysis or laser diffraction
analysis)
Methodology
Saucier’s criteria:
The medium gravel pack size should be about 5 to 6 times the mean formation sand
size.
Tiffin et al’s Screen criteria:
Uniformity coefficient (D40/D90), sorting coefficient (D10/D95) and mass fraction of fines
(smaller than 44um) are used for Tiffin’s screen criteria as follows:
• Standalone screens can be used if D10/D95 < 10, D40/D90 < 5 and fines fraction <
5%wt. WWS used when D40/D90 < 3 and fines fraction < 2%wt. Premium screens
should be used when 3 < D40/D90 < 5 and 2wt% < fines fraction < 5%wt.
• Gravel Packing should be used if D10/D95 > 10, D40/D90 > 5 and fines fraction >
5%wt.
Price and Smith Method
Refine the selection process and further the choice as to whether or not to go gravel
pack or standalone based on follows:
• If D50 > 75um and D10/D95 > 10 or D40/D90 > 5 or fines fraction > 5%wt, gravel
packing is default except for
(1) Non-subsea oil or gas producers with short well life (i.e. less than 3-5
years).
(2) Low rate oil (less than 10BFPD/ft of net interval) non-subsea
producers with high net to gross (greater than 80%)
• If D50 > 75um and D10/D95 < 10 and D40/D90 < 5 and fines fraction < 5%wt,
standalone is default except for
(1) Low rate oil/gas producers of Subsea or non-subsea with continuous
shale sections having partial/no hole collapse and net/gross less than
80% and annular/pipe area greater than 1.25.
129
(2) High rate oil/gas producers with partial/no hole collapse and net/gross
less than 80% regardless of subsea or not and the annular/pipe area
ratio.
(3) Oil/gas injectors with net/gross less than 80% and annular/pipe area
ratio greater than 1.25.
(4) Gas injectors with net/gross less than 80% and annular/pipe area ratio
less than 1.25
130
SC-003 Sand Settling Test
Introduction
The suspension behavior of gravel in the carrying fluid is one of the very important
factors (other factors as fluid rheology, leak-off behavior, formation damage) to affect
the quality of gravel pack treatment. Generally the gravel settling test is performed at
the surface conditions. But here we describe a procedure on how to test the sand
settling properties at elevated temperature.
500-mL graduated cylinder with cap for less than 100C
HT bottles with cap for greater than 100C
Plastic funnel
Balance
Waring blender
Water bath/oil bath
Procedure
1. Weigh out the required particle concentration.
60 × ppa
Wt of Sand =
0.046 × ppa + 1
2. Prepare the fluid.
wt of sand
Fluid volume = 500 −
2.62
3. Mix the slurry (adding gravel into the carrying fluid) with high speed until uniform
dispersed.
Following Testing For BHT Less Than 100C

4. Pour the slurry into a 500 mL graduated cylinder using a plastic funnel up to the
500 ml mark.
5. Place the cylinder with cap into a waterbath.
6. Measure the temperature of the fluid until temperature reaches BHT.
7. Take out the capped cylinder and shake vigorously during as short duration as
possible.
8. Place the slurry back to water bath and record graduations of clear liquid every
five minutes
9. Calculate % sand settling.
clear volume
% settling =
500 − total sand volume
131
Following Testing For BHT Greater Than 100C

10. Pour the slurry into a marked HT bottle using a plastic funnel. Cap the bottle.
11. Place the slurry with bottle in heating oil bath for 15-20 minutes to reach BHT.
12. Take out the capped slurry and shake vigorously during as short duration as
possible wearing thermal gloves.
13. Place the slurry back to oil bath and record graduations of clear liquid every five
minutes
14. Calculate % sand settling.
clear volume
% settling =
500 − total sand volume
132
SC-004 K300 Sand Consolidation Testing

Introduction
In the loose sand water-sensitive formations (either gas or oil wells), we generally
recommend furan resin treatment (K300) to consolidate the sand/fines migration. By
acid catalyst, the resin polymerized at BHT cures to a hard plastic material to bond
the sand grains together and further to control the migration of loose sand and fines
from the formation into the wellbore. Following procedures describe a method on a
QA/QC testing of K300 performance.
Syringe with 1” ID/100 mesh screen
Plastic graduated cylinder
Aging cell to contain the capped syringe
Oven or water bath/Stopwatch
DI water/K300/W58, KCl/15%HCl/HEC fluids I, II, III
Procedures
• Remove plunger from syringe.
• Place a pre-cut 100 mesh screen into the syringe tip. Add 20-25ml of S100 into
the syringe.
• Wet sand with 2% KCl + 0.5% W59. Volume is four times of K300 volume.
Syringe 30ml K300 on sand top and plunge it slowly through the sand plug.
• Add displacement fluid HEC I, II, III step by step on the sand top and plunge them
slowly through the sand plug. Volume should be 4 times of K300 volume.
• Add 15% HCl (with inhibitor), volume four times of the volume of K300.
• Let remain under room condition for 15 minutes.
• Place the capped syringe in oil-fill aging cell applying 500psi pressure to an oven
at BHST (for greater than 100C) or to a water bath (for less than 100C), heating
about 12-48 hours at desired BHST.
• Cut the plug with syringe coating to 1” height using a hacksaw.
• Remove the sand plug carefully from the syringe sleeve.
• Measure the core dimensions.
• Crush the core using a hydraulic press and record the crushing loading.
• Calculate the UCS by
UCS (PSI) = LOADING/CORE X-SECTIONAL AREA
133
SC-005 SANDLOCK V Preparation Procedures

Introduction
SANDLOCK V is a resin-coated-gravel packing technique which gives us good
compressive strength with high permeability and low resin content and short shut-in
time. The limitation are for low temperature application (less than 225F), shorter
treatment interval and in-compatible with mud acid.
Plastic container
Heating source
KCl/J164/M45/L41/W27/K230B/K235B/K187/sand
Procedures
• Add 500ml of fresh water in a plastic container.
• Add 12 g KCl and mix.
• Add 0.5ml M45.
• Add 4.3 g J164. Add quickly but do not dump. All J164 must be added before its
hydration starts to obtain dispersion of the resin. Continue mix until fully
dispersed.
• Add 1.2 g L41 to raise the pH above 6.5. Add NaHCO3 if pH is not getting greater
than 6.5 after adding L41.
• Mix until max viscosity obtained.
• Check Fann35 at 75F at 100rpm (170sec-1), should be 180-290cp.
• Add 5ml W27 and mix.
• Add gravel and mix for 5 minutes.
• Add 75ml K230B and mix.
• Add 25ml K235B and mix.
• Add 2.5ml K187 and mix.
• Place the slurry in a heating source at BHST until the slurry set.
134
WC-001 Test Procedures for OrganoSEAL-R Working Time Determination

(greater than 100C)
Introduction
OrganoSEAL-R is mainly used for water shut-off although can also be used in place
of cement squeeze to fix the casing bon failure. The application temperature is up to
250F and can penetrate deeper into the formation due to the low molecular weight.
Controlled working time and simple mixing/metering in the field are other advantages
of this fluid. Following procedures are the general methods used in the lab to
determine OrganoSEAL-R working time.
J464/J524/J525/J491
HT bottle
Oilbath in oven
Syringe
One inch luer filter holder
Whatman 54/540
Magnetic stirrer
Thermal gloves
Stopwatch
Procedures
FOLLOWING PROCEDURES FOR >100C
(1) Using DI water, add stabilizer J464. Next add gelling agent J491 slowly while
stirring and continue to hydrate until fully hydrated.
(2) Add J524 and mix thoroughly, followed by J525.
(3) Fill (3/5 of the total volume) the HT glass bottle with the gel and tighten the cap.
(4) Place the glass bottle in a preheated oil bath in a static oven set at BHIT.
(5) Visually observe the change in color and flow of the gel (by tilting the glass bottle)
every half an hour.
135
FOLLOWING PROCEDURES FOR <100C

• Using field mix-water, add J464 if required. Next add gelling agent slowly while
stirring and continue to hydrate for at least on hour on the magnetic stirring plate.
• Prepare 10% solution of J525 and add J524/525 to mix for a minute.
• Add activator if required at this stage.
• Fill the syringe with solution and attch a luer filtration unit containing a appropriate
filter paper. (54 for >300mD, 540 for <300mD)
• Inject a small amount of fluid through the filter, noting the force needed.
• Place the plastic tip over the tip end of the filter holder to prevent gel from
skinning over.
• Place the assembly in the preheated oven and start the stopwatch.
• Remove the assembly from the oven at proper intervals (10 minutes), each time
forcing the fluid through the filter to observe the force required.
• Note the elapsed oven time when the fluid can no longer be forced through the
filter, this is the gel working time.
136
Marathon Gel Code

A No detectable gel formed: The gel appears to have the same viscosity (fluidity)
as the original polymer solution and no gel is visually detectable.
B Highly flowing gel: The gel appears to be only slightly more viscous (less fluid)
than the original polymer solution.
C Flowing gel: Most of the obviously detectable gel flows to the bottle cap upon
inversion.
D Moderately flowing gel: Only a small portion (about 5 to 15%) of the gel does
not readily flow to the bottle cap upon inversion-- usually characterized as a
“tonguing"gel (i.e., after hanging out of jar, gel can be made to flow back into
bottle by slowly turning bottle upright).
E Barely flowing gel: The gel can barely flow to the bottle cap and/or a significant
portion (>15%) of the gel does not flow upon inversion.
F Highly deformable nonflowing gel: The gel does not flow to the bottle cap upon
inversion.
G Moderately deformable nonflowing gel: The gel flows about half way down the
bottle upon inversion.
H Slightly deformable nonflowing gel: The gel surface only slightly deforms upon
inversion.
I Rigid gel: There is no gel-surface deformation upon inversion.
J Ringing rigid gel: A tuning-fork-Iike mechanical vibration can be felt after

tapping the bottle.
137
WC-002 Test Procedures on Evaluation of OrganoSEAL-R Shut-off Effectiveness
Introduction
A laboratory procedure of evaluating water shut-off effectiveness at the bottom hole
conditions is important on the field job quality. Following procedures use core flow
tester and formation damage tester to simulate Organoseal-R treatment
effectiveness at downhole condition.
FRT/SCR FDT
OrganoSEAL-R additives
Procedures
(1) Dry the core plug in oven for overnight and check the initial N2 permeability after
core preparation.
(2) Vacuum saturate and then preserve the core plug in 2% KCl solution.
(3) Wrap the core sample with Teflon tape, mount it in the FRT sample holder.
(4) Apply 500 psi confining pressure and 100 psi backpressure.
(5) Flow 2% KCl at 8 cc/min to fill up the line. Once flow breakthrough, flow 1 cc/min
of 2% KCl until permeability reading is stable.
(6) Using the modified HTHP baroid cell, reverse the core plug to treatment direction
and place two PV mls of Organoseal R above the core. Cover the cell with end
cap, place it in the HP/HT jacket on the stand and connect to the N2 line directly.
Heat the HTHP cell up to BHIT. Open the bottom valve and apply the N2
pressure up to 100psi on the top monitoring the volume of the filtrate collected
over time duration from the beginning of the flowing to first drop of gel flowing out.
(7) Once seeing the first drop of the gel, close both top and bottom valves and shut-
in at 100 psi and BHST F for desired time duration.
(8) Cool down the heater jacket and bleed off the pressure. Take the core off the cell
and scrap off the gel on the core face.
(9) Check N2 permeability with the wet core plug.
(10) Vacuum saturate the core in 2% KCl for 24 hours prior to checking liquid
permeability with FRT
(12) Calculate the retained permeability using initial and final permeability as
following.
Kretained = Kfinal/Kinitial x 100
138
WC-003 DGS Gel Working Time Determination
Introduction
DGS solution is particularly useful for treating production and injection problems that
require reduction of
permeability on the order of tens feet around the wellbore. It is a permanent plugging
gel which has the
following advantages
(1) Effective permeability reduction more than 90%.
(2) Deep penetration due to very low viscosity before gel set and not reactive with
reservoir rock, formation minerals and fluids and tubular.
(3) Rapid gel set from low viscosity to rigid gel.
(4) Shear insensitive and easy mixing.
QA/QC the gel working time in the field by in-situ field chemicals and water/brine
before the job are extremely important for a right field job DEE.
Following tests are generally performed in the lab to design the DGS system
(1) Gel working time at BHST to get greater than 8 hours gel time.
(2) Gel extrusion test to semi-quantitatively evaluate the extrusion pressure gradient.
Field water
Field and lab KCl
J467/J470 (both lab chemicals and field chemicals)
100ml high temperature bottles
heating oven
pH meter
Static FDT
Test Procedures
Gel Working Time Determination
(1) Run water-support software to get formulation and lab-mixing amount.

(2) Place water into the 100ml bottle, shake to dissolve and check pH.
(3) Add KCl as designed amount to dissolve and check pH.
(4) Add required amount of J467 and shake to dissolve, measure pH, which is about
4.0-4.5.
(5) Add the desired amount of J468 activator if necessary, shake to dissolve.
(6) Add J469 and J470 to shake 5-10 minutes for complete dissolving. Check pH,
which is supposed to be about 4.5.
139
(7) Place gel in high temperature bottles and place it in the preheated oven.
Periodically check pH and gel shape by turbidity, viscosity and Marathon gel code
until a change of gel appearance from clear to turbid, at which point the pH of the
fluid is supposed to be about 5.5 to 6.0.
Typical DGS Gel Shape Before (the left) and After Crosslinking (the right)
Gel Extrusion Test
(1) Vacuum saturate the appropriate core plug as properties described in core
preparation.
(2) Mix the DGS fluid as designed by above tests.
(3) Place the core plug in the modified Baroid cell and add 80-90mls of DGS fluid on
the cell top.
(4) Apply pressure on the top to displace the gel through the core plug until amount
of gel flowing out of the cell.
(5) Stop flowing, shut off both end valves and heat the cell up to BHST.
(6) Shut in the period of time as required.
(7) Take off the assembly and place 2% KCl on the top of the core.
(8) Close end valves and heat up the cell to BHST.
(9) Open the bottom valve with 100psi back pressure and 100psi on top. Open the
top valve and increase the top pressure stepwise.
(10) Record the pressure on the top while the flow starts being initiated. (see flow
out from bottom)
(11) Calculate the gel extrusion pressure as psi/ft.
140
SECTION 6 ANALYTICAL METHODS
AM-001 Water Analysis

Introduction
The oil industry has used water analysis for such purposes as quality control,
formation identification, compatibility studies and environmental evaluations.
The following procedures are developed for our laboratory use. Make sure that these
procedures may not be applicable for the use of other purposes.
(1) pH (meter), Specific Gravity (SG bottle method) and turbidity (HACH method)
pH meter and calibration fluids
SG bottle
Balance
Filtering apparatus and accessories (filter paper, vaccum pump and funnel
assembly), optional
DI water
Water sample
Test Procedures
• Filter the sample if not clear by observation. Use the filtrate for further analysis.
• Calibrate pH meter as required in the pH meter manual.
• Shake the water sample for homogenity. Insert the probe into the water sample.
• Read the pH after the reading is stably shown on the meter screen. Record the
pH and temperature.
• Weigh the empty SG bottle and record. (W1)
• Fill the bottle with DI water and cap it until water out of the cappilary.
• Weigh the bottle containing DI water. (W2)
• Clean bottle with water sample three times, fill it with water sample and cap it.
• Weigh the bottle containing water sample. (W3)
• Clean everything up with DI water.
• Switch on the HACH2000 spectrophotometer and enter the method # 750.
• Adjust the wavelength to 450nm for test.
• Fill in two clean sample cells with 25ml water sample and 25ml DI water
respectively.
• Insert DI water sample cell into the cell holder and close the shield.
141
• Press “ ZERO ” zero the machine.

• Place the sample cell into the holder and close the shield.
• Press “READ/ENTER” to get the FTU water turbidity.
• Clean up the cells and turn off HACH2000.
Calculation
S.G. of water sample = (W3 - W1) / (W2 - W1)
142
(2) Alkalinity (indicator method)

Erlenmyer flask
Buret
Pipette
Standard HCl solution (0.1014N)
Phenolphthalein indicator (0.5gphenolphthalein dissolved in 50ml 95% ethyl alcohol
or isopropyl alcohol and dilute to 100ml with DI water)
Methyl purple inndicator solution
Water sample
Test Procedures
• This analysis should be made immediately after determining the pH in order to
minimize errors due to decomposition of the bicarbonate.
• Transfer an undiluted sample, usually 25 cubic centimeters, into an Erlenmeyer
flask and add 2-5 drops of phenolphthalein.
• Titrate with standard HCl acid solution while stirring to the phenophthalein end
point and record this value as P.
• Add 3-4 drops of the methyl purple indicator solution and continue the titration
with stirring to the point at which the color changes. Record the total volume of
acid used in the titrating both indicators as T.
Volume of standard acid corresponding to

results HCO3- CO32- OH-
P=0 T 0 0
P ≤ 0.5T T – 2P 2P 0
P = 0.5T 0 2P 0
P ≥ 0.5T 0 2 (T - P) 2P - T
P=T 0 0 T
Calculation
mg/l HCO3- = (ml acid × N acid × 61 × 1000) / ml sample
mg/l CO32- = (ml acid × N acid × 30 × 1000) / ml sample
mg/l OH- = = (ml acid × N acid × 17 × 1000) / ml sample
143
(3) Chloride (Mohr method)

Erlenmyer flask
Buret
Pipette
0.02N nitric acid
Standard silver nitrate solution
Potassium chromate indicator
Test Procedures
• Pipette 25 cubic centimeters of sample into the flask. Add 2-3 drops of
phenolphthalein solution. If the indicator turns pink, add 0.02N sulfuric or nitric
acid drop by drop, while stirring, until the color is discharged.
• Add and 2-5 drops of potassium chromate solution.
• Stir continuously while adding standard silver nitrate solution drop by drop from
the buret until the color changes from yellow to orange red and persists for 30
seconds.
• Record the number of cubic centimeters of silver nitrate solution required to reach
the endpoint.
Calculation
Chloride, mg/l = mls of AgNO3 solution × N × 35500 / mls of sample
144
(4) Calcium and Magnesium (Compleximetric method)

Erlenmyer flask
Buret
Pipette
Triethanolamine
KOH solution
NH4OH-NH4Cl buffer solution (pH=10)
Standard EDTA solution
Murexide indicator
Erichrome Black indicator
Test Procedures
• Pipette 25 cubic centimeters of sample into the flask. Add 2-3 drops of
Triethanolamine to prevent Fe interference. Add KOH solution drop by drop until
the pH reaches about 14.
• Add murexide indicator to get clear pink color.
• Stir continuously while titrating with standard EDTA solution until the color
changes from pink to purple.
• Record the number of cubic centimeters of EDTA. (Aml)
• Pipette another 25 cubic centimeters of sample into the flask. Add NH4OH-NH4Cl
buffer solution to get pH=10.
• Add Erichrome Black indicator to get wine color.
• Stir continuously while titrating with standard EDTA solution until the color
changes from wine to blue.
• Record the number of cubic centimeters of EDTA. (Bml)
Calculation
Ca, ppm = A × 40.08 × N of EDTA × 1000 / 25
Mg, ppm = (B - A) × 24.3 × N of EDTA × 1000 / 25
145
(5) Sulphate, Barium, Iron and Potassium (HACH method)

HACH2000 with accessories
DI water
Sulfaver Reagent Powder Pillow, for SO42-
Bariver 4 Reagent Powder Pillow, for Ba2+
FeroVer Iron Reagent Powder Pillow, for Fe2+/Fe3+
Potassium I/II/III Reagent, for K+
Test Procedures
• Switch on the HACH2000.
• Enter the stored program number 680 for sulphate, 20 for Barium, 265 for for iron
and 950 for potassium.
• Rotate the wavelength dial until the display shows 450nm for sulphate and
barium, 510nm for iron and 650nm for potassium.
• Press READ/ENTER.
• Pour 25ml of sample into the sample cell.
• Add the contents of reagent powder pillow to the sample cell (the prepared
sample). Swirl to dissolve.
• Press SHIFT TIMER.
• When the timer beeps, fill another sample cell (blank) to 25ml of sample. Place it
into the cell holder and close the light shield.
• Press ZERO
• Within a few minutes after the timer beeps, Place the prepared sample into the
cell holder. Close the light shield.
• Press READ/ENTER.
• Record the reading.
• Dilute the sample if the reading flashes (over limit) and repeat the above
procedures.
Calculation
Mg/l = reading × dilution factor
146
(6) Sodium (calculation method)

mg/l of Na+ = 23 × (A/35.5 + B/61 + C/60 + D/17 – E/56 – F /137 – G/24 – H/40 –
I/39)
where
A: mg/l of chloride
B: mg/l of bicarbonate
C: mg/l of carbonate
D: mg/l of OH-
E: mg/l of iron
F: mg/l of barium
G: mg/l of Mg 2+
H: mg/l of Ca 2+
I: mg/l of K+
147
AM-002 Cloud Point Determination

Introduction
The following procedure describes a method for determining the cloud point of a
transparent fluid.
Test jar, clear glass, cylindrical form, flat bottom, 30mm Diameter × 120mm Height.
The jar should be marked with a line to indicate the sample height of 2 - 2.25 inch
above the inside bottom.
Thermometer, range to accommodate the test
Cork, fit with jar with a hole in the center to accommodate the thermometer
Jacket, ID 9mm-12mm greater than OD of jar, water-tight cylinder with a flat bottom.
Disk, ¼ inch thick cork or felt disk, OD=ID of jacket, keep test jar from the bottom of
jacket
Gasket, sitting between jar and jacket to keep the jar from touching the walls of the
jacket
Cooling Bath,
Components lowest temperature
Ice water 50oF
Crushed ice and NaCl 10oF
Crushed ice and CaCl2 -15oF
Dry ice/Acetone -70oF
Test Procedure
• Bring the fluid to be tested to a temperature of at least 14oC above the estimated
cloud point.
• Pour the fluid into the test jar to the marked level.
• Closed the jar tightly by the cork with thermometer. Adjust the position of the cork
and the thermometer so that the cork fit tightly, the thermometer and the jar are
coaxial and the thermometer bulb is resting near the bottom of the jar.
• Place disk in the bottom of the jacket. Place ring gasket around jar (25mm from
the bottom). Keep all surfaces of jacket, ring and jar clean enough. Insert jar into
the jacket.
• Maintain the cooling bath temperature at –1oC to +2oC. Keep whole assembly
vertical and jacket immersed into the cooling medium.
148
• For each 1oC temperarure drop, remove the jar quickly from the jacket without
disturbing the fluid, inspect the cloud and replace back to jacket. This complete
process should be finished in less than three seconds.
• When the fluid doesnot show cloud point when temperature reaches the limit of
this cooling bath, transfer the jar to another jacket in the second bath maintained
at a tempearture of –18oC to –15oC, do not transfer the jacket.
• Continue the above process until a distinct cloudiness or haze comes up in the
fluid at the bottom of the test jar, reacord the reading of the test thermometer as
the cloud point.
149
AM-003 Methylene Blue Index Determination

Introduction
The methylene blue test measures the total exchange capacity of the clay system.
(generally a little less than CEC) The method is mainly developed for drilling fluids,
but it can be effectively applied to aqueous dispersions of powdered clays, cores, drill
cuttings and molding sands.
Results are expressed as meq/100g sample. Typical MBI values for clay minerals are
listed below.
minerals MBI (meq/100g of sample)
Reactive water sensitive shale 25
kaolinite 3-15
mica 10-40
montmorillonite 80-150
attapulgite 15-25
chlorite 10-40

150ml beaker
50ml burette
20ml and 2ml syringes
glass rod
water bath
magnetic stirrer
Whatman No.1 filter paper
Balance
Methylene blue solution (1ml=100meq)
3% H2O2 solution
5N H2SO4
DI water
Test Procedure
• Weigh accurately 1 gram of sample into 150ml beaker.
• Add 15ml 3% hydrogen peroxide, 15ml od DI water and 1ml of 5N sulfric acid.
• Place the beaker in a boiling water bath and heat gently for 15 minutes.
• Cool down the beaker, the slurry is titrated against a solution of methylene blue.
150
• Fill the burette with methylene blue solution and the beaker of slurry is tirred
using a magnetic stirrer.
• Take the initial burette reading and add the methylene blue in 1 ml increments.
• After each increment, allow the slurry to stir for 15 seconds.
• Use a glass rod, drop a sample of the mixture on a fast filter paper. The sample
will produce a clear halo around a dark blue central spot. As the end point
reached, the halo will become a pale blue.
• Allow the slurry to stir for a further minute and place another sample on the filter
paper. The end point is considered to be reached if the pale blue remains.
• Record the mls of methylene blue being used.
Calculation
Meq/100g of tested sample = mls of methylene blue used/grams of tested sample
151
AM-004 Vapor Pressure Measurement

Introduction
This method, which is called Reid method, describes a means of determining the
vapor pressure of petroleum products. This method offers the type of data commonly
requested by the field. Refer to ASTM D323-82 for more precise and absolute vapor
pressure measurement.
Safety
Keep heat and ignition away from the test.
Tested sample
Water bath, adjustable from 100-140F
Reid vapor pressure tester, refer to ASTM232-82 for detail
Test Procedure
• Sample should be handled with diligence to minimize vapor loss.
• Unscrew the testing chamber of its mid-section and inspect the O-ring seal.
• Transfer 25-30ml of sample to the bottom half of the testing chamber, then
quickly screw the upper and lower halves together.
• Immerse the apparatus into the water bath and start heating. Heat bath slowly so
the sample temperature is close to the bath temperature.
• Record vapor pressure of the sample when the temperature is 100F.Note the
exact temperature and pressure when making a reading. Be sure to shake the
test chamber vigorously before each reading to ensure that the validity of the
sample has been maximized.
• Continue heating and read the vapor pressure again when the bath temperature
is 130F. Note the exact temperature and pressure.
• Discard the sample and thoroughly wash the apparatus with water.
Calculation
Plot pressure vs. temperature of the data collected and extrapolate to obtain the
exact pressure at 100F and 130F for reporting.
152
AM-005 Determination of Asphaltenes and Paraffin Wax

Introduction
This method is not a method to determine the amount of materials which belong to
these two catecaries of materials. It is just used to determine the approximate
amount of high MW of compounds which are called “asphaltenes” and” paraffins”
which might precipitate from oil or help to stabilize emulsions.
Safety
Organic solvents are used in the testing, extra caution needed for these flammables
and poisonous
Insulated gloves/clothing for dry ice
Centrifuge and accessory
Flask/beakers
Magnetic stirrer/bars
Steam bath
Acetone/pentane/toluene/dry ice
Procedures for asphaltene content
• Add 10g oil (W0) and 90ml pentane in a pre-weighed centrifuge tube (100ml). W1
• Cap the tube and shake vigorously, centrifuge at 2000rpm for 5 minutes.
• Decant and discard the clear part.
• Repeat above steps until the colorless of the pentane solution on the top.
• Final washing the tube and decanted and air-dry until no ordor of n-pentane is
noticeable.
• The tube is then dried in oven at 200F for 30 minutes, cool down and re-weigh.
W2
• Calculate asphaltene content as wt% = (W2 - W1)/W0 × 100%
Procedures for paraffin content
• 5 grams of oil (W0) is added into a 150ml beaker. Add 80ml acetone.
• Stir the mixture vigorously for 5 minutes.
• Transfer the mixture to a pre-weighed centrifuge tube (100ml) W1
• Place the tube in a dry ice/acetone cooling bath to precipitate for 10 minutes.
• Centrifuge and discard the acetone.
• Repeat above steps until discarded acetone is colorless.
• Dry the tube in 200F oven for 10 minutes. Allow the tube to cool down to room
condition and weigh. W2
153
• Add 50ml pentane to the residue in the sample beaker.
• Stir vigorously for 5 minutes and let the solids settle, centrifuge if necessary.
• Extract sample with 50ml aliquots until pentane is colorless.
• Combine all pentane extractions in a beaker (pre-weighed W3) and evaporate
pentane using a steam bath. Re-weigh the beaker plus residue. (W4)
• Calculate low MW paraffin as A (wt%) = (W2 – W1) /W0 × 100%
• Calculate high MW paraffin as B (wt%) = (W4 – W3) /W0 × 100%
• Calculate paraffin content as C (wt%) = A + B
154
AM-006 Scale/Solids Identification by XRD/Solubility/Water Analysis/EDAX

Introduction
The quantitative composition information on the downhole scale/solid/slurry sample is
very important in identifying the types and mechanism of formation damage and
recommendation of right treatment. This procedure describes a method of sample
identification by a combination use of different analytical instrumentals such as XRD,
SEM/EDAX and Wet chemistry.
XRD
ESEM/EDAX
Apparatus/reagents for Water analysis in 06-001
Solubility apparatus in 02-019
Procedures
• Grind the sample to less than 500um if solid fragment. (physical observation for
pre-screening)
• Pre-weigh two parallel unknown sample (5 grams each) and disperse it in two
pre-weighed beakers containing 100ml DI water and 100ml toluene respectively.
• Stir vigorously to get complete dispersion of the sample in solvent. (sample oil-
wet of not dispersing in water, otherwise water-wet), Add surfactant if necessary
to disperse.
• Run solvent (water and toluene) solubility as described in solubility method. The
content of oil ingredients or water soluble ingredients will be the solubility of
sample in each solvent (organic and inorganic content).
• Use the sample residue after toluene solubility to run water solubility (total
content of water soluble salt)
• Analyze the filtrate from water solubility test by water analysis methodology.
(content of each water soluble salt)
• Check the viscosity/trubidity of the water soluble part if viscous solution observed
to correlate the concentration of hydrated water soluble polymer (total content of
water soluble polymers).
• Further Analytical methods for analyzing content of different water soluble
polymers are used if necessary.
• Analyze the residue part from the water solubility test by XRD (minerals
presented, EDAX/elemental information)
155
• Combination of EDAX quantification (Phoenix) and XRD quantification (Siroquart)

is used in determining the content of each minerals and other compounds
presented in the unknown sample.
Philips ESEM/EDAX System
Bruker D5005 Powder Diffraction Unit
Wet Chemistry and HACH Spectrophotometer
Potential Scale Problem
156
Crude analysis Oil smelly? of scale
solid/slurry
Light Wax Asphaltene yes, to no,
to oven dry and then go to

Hydrocarbon check water/toluene dispersivity XRD/EDAX
combinational analysis to treatment water dispersive, to oven dry

toluene dispersive, to to treatment
recommendation to XRD/EDAX combinational analysis semi-quantitative toluene
recommendation
water soluble polymer if physically noticed solubility
methanol
clean
and then oven dry
to XRD/EDAX
to treatment recommendation
Schematic Scale Analysis Procedure
157
SECTION 7 LABORATORY SAFETY
LS-001 MEA WELL SERVICES LABORATORY AUDIT
Enter score (0 to 3) or NA (not applicable)

0 1 2 3 Score
1 - Laboratory building facilities
Access to the lab Poor Med Good Excel.
Is there enough space for all the lab equipment Poor Med Good Excel.
Is the lab clean Poor Med Good Excel.
Is the lab office separated from the lab No yes
Lab office condition Poor Med Good Excel.
Do visitors have to pass through the lab to get to the lab office Yes No
Changing room facilities Poor Med Good Excel.
Special enclosure for high pressure equipment as per SLPM 24 Poor Med Good Excel.
Water/sink / draining board Poor Med Good Excel.
Air pressure system Poor Med Good Excel.
Separate store room No Yes
Store room condition Poor Med Good Excel.
Does the lab have adequate ventilation Poor Med Good Excel.
Vapour Gas extractors and suitable filters Poor Med Good Excel.
Subtotal 0
2 - Safety
Safety exit / sign post None Some Most All
Safety instructions / sign post None Some Most All
Emergency lighting ? No Yes
Are safety spectacles available for visitors ? No yes
Are there copies of MSDS in the lab for all chemicals, including 3rd party chemicals ? None Some Most All
Does the lab have the required safety equipment 0-10% 11-50% 51-90% >90%
Is there a copy of SLPM 24 available in the lab ? No Yes
Subtotal 0
3 - Lab equipment
Does the cement lab have the required cementing lab testing equipment 0-10% 11-50% 51-90% >90%
Does the stimulation lab have required stimulation lab testing equipment 0-10% 11-50% 51-90% >90%
Is the lab equipment clean and in good condition 0-10% 11-50% 51-90% >90%
Is the equipment regularly maintained Never Sometime Often Always
Is the equipment regularly calibrated Never Sometime Often Always
Does the lab have enough spare parts 0-10% 11-50% 51-90% >90%
Subtotal 0
4 - Sample storage
Are the additive samples labelled with the correct hazard warnings? 0-10% 11-50% 51-90% >90%
Do the additives have a record of the sample date and Mato number ? 0-10% 11-50% 51-90% >90%
Are the additives stored in adequate containers ? None Some Most All
Are rig samples labelled with the date, rig name, silo number, well number, client ? None Some Most All
Are cement samples stored in airtight drums ? No Yes
Is there a log kept for tracking samples ? No Yes
Subtotal 0
5 - Record keeping
Are copies of worksheets filed and easily available for reference ? None Some Most All
Are lab reports filed and easily available for reference ? None Some Most All
Are lab reports available on the location server ? No Yes
Are the lab databases available on the location server ? No Yes
Is there a log of equipment maintenance ? No Yes
Is there a log of equipment calibration ? No Yes
Is there an inventory of spare parts ? No Yes
Is there an inventory of additives ? No Yes
Is there an inventory of lab equipment ? No Yes
Subtotal 0
159
6 - Design & planning

Is LabDB installed on the lab computer and currently used No Yes
Are the calculations required for planning a test program performed accurately ? 0-10% 11-50% 51-90% >90%
Is there a copy of the latest edition of API Spec 10 available ? No Yes
Are other relevant API publications available eg API RP56 for frac sand QC ? No Yes
Do Lab Staff participate in the job design ? ( BHCT determination etc…) Never Sometime Often Always
Is the Lab responsible for sampling of additives / cement at the base Never Sometime Often Always
Is the Lab responsible for requesting offshore / rigs samples before the job Never Sometime Often Always
Are the tests confirmed with cement / additives / water sample from the rig before job Never Sometime Often Always
Are the samples from rig sent in a dedicated container Never Sometime Often Always
Are there copies of the business line manuals in the lab ? No Yes
Do Lab Staff take part in the daily operation meeting ? Never Sometime Often Always
Does a Lab representative visit the client along with FE ? Never Quarterly monthly weekly
Does the Lab have a daily update on rig operation Never Sometime Often Always
Does the Lab have access to the web ? No Yes
Subtotal 0
7 - Implementation & monitoring
Is a Lab Analysis Request (LAR) submitted for all testing ? None Some Most All
Does the Lab have enough skill to modify fluid designs if initial results are not
None Some Most All
satisfactory ?
Are final reports submitted to the LAR originator in plenty of time ? 0-10% 11-50% 51-90% >90%
How many times did anyone from the Lab assist at the wellsite last year ? Never 1 job 2-3 jobs >3 jobs
Does the Lab get feedback on any job which was tested in the lab ? Never Sometime Often Always
Do Lab Staff supervise/assist the blending of CemCRETE components No Yes
Subtotal 0
160
8 -Personnel
Are there enough LT's to cope with the lab workload ? Never Sometime Most Always
Do any of the Lab Staff require further specialised training ? All Most Some None
Are the Lab Staff properly motivated to do the job ? Never Sometime Often Always
Do the Lab Staff work with the required precision to do the job ? Never Sometime Often Always
Can the Lab Staff work without daily supervision ? Never Sometime Often Always
Do the Lab Staff have the skills required to train SS's and FE's (SCDP modules) ? No Yes
How many courses/training sessions were attended last year at the district level None 1-2 3-4 >4
Did any LT attend a training course at region level in the last 12 months ? No Yes
Is InTouch used ? No Yes
How many InTouch submissions did the Lab post last quarter ? 0 1 2 3
Is Intouch used for document search and retrieval ? No Yes
How many times was MEA CSL lab asked for help in the last year ? Daily Often Rarely Never
Is this Lab happy with the help given by MEA CSL ? Never Sometime Often Always
Subtotal 0
Total
Score 0 points - of - 225
161
LS-002 MEA CSL WORKING ALONE PROCEDURES
PURPOSE
This procedure outlines the responsibility and activities required to ensure the safety of personnel required to work alone in the
Laboratory.
RESPONSIBILITIES
The Lab manager is responsible for ensuring a risk assessment has been conducted to identify additional control measure that may
be necessary when employees are required to work alone and for providing additional traning and equipment when required.
The lone worker is responsible to bring to the attention of their supervisor any unsafe conditions and hazards associated with the
tasks they are required to conduct when working alone.
Supervisors are responsible to ensure that the tasks are not conducted by personnel working alone, where it is not safe to do so.
PROCEDURE
An assessment of the risks of working alone will confirm if the work can actually be done safely by one unacompanied person. This
will include the identification of hazards, for example, Lab equipments, goods, substances, environment, atmosphere etc.
Employees will be given all necessary information, instruction, training and supervision to enable them to identify the hazards and
appreciate the risks involved with working alone. Empployees are required to follow the safe systems of work in place, which will
include the provision of first aid, communication procedures and awareness of emergency procedures. All employees are required to
co-operate with these efforts to ensure safe working and to report any concerns to management.
Apart of employees being sure that they are capable of doing the job on their own, the three most important points that have to be
considered are:
• The person working alone has full knowledge of the hazards and the risks to which they are being exposed.
• The lone worker knows what to do if something goes wrong.
• Someone else always knows the whereabouts of a lone worker and what they are doing.
Additional equipment may be required to ensure personnel working alone can performed their tasks safely.
162
Lone worker Risk Assessment
A risk assessment must be conducted for operations involving lone workers:

1. Assess the hazards and risks involve in the work.
2. Assess the working environment, are there any limitations imposed on the worker.
3. Develop and implement safe working arrangements to ensure that the risks are either eliminated or adequately controlled.
4. Ensure the lone worker is adequately trained and instructed in the necessary procedures for lone working, including
emergency procedures.
5. Ensure someone always knows the location and the operations being performed by the lone worker and this person is notified
when the operation has been completed.
The main issues, which need to be addressed as part of ther assessment process, are:
• Access and exit from the Laboratory

• Forseeable emergency, e.g. fire or ill health.
• The process or work performed and the risks associated.
• The fitness and medical history of the personnel involved.
• Use of dangerous equipment or machinery.
• Use of hazardous substances or chemicals.
• Working in confined spaces.
• Exposure to gasses or lack of oxygen.
• Training required for emergencies, or unusual situations.
• Th need for manual handling operations.
The following arrangements shoould be considered:
• Supervisors to visit regularly and monitor people working alone.
• Lone workers to check-in at regular intervals by phone.
• Informed the suprvisors when the job has been completed.
162
LS-003 MEA CSL TYPICAL STIMULATION CHEMICALS HANDLING GUIDELINES
Code Description Handling Spillage First aid Fire Remarks

A201 Organic acid • Lab coat • water flush a Water fog.Alcohol foam • Acids are corrosive.
L001 • Glasses • neutralize with soda CO2/Dry chemical • Lab operating in vent-hood
L041 • Gloves • cleanup after pH 6-8 • Remember organics always
L400 • Respirator cause fire if not operating
HCl Inorganic acid • SCBA • water flush a No need properly.
H2SO4 • Goggles/mask • neutralize with lime • Inorganic acid cause serious
HF • Imperious gloves • go plastic container burns (acid hydration)
H3BO3 • Acid resistant suit/boot • HF highly reacts with glass.
• 98%H2SO4 removes water and
cause charring.
J059 Bases • SCBA • scoop to container a No need • cause severe skin burns if
M002 • Goggles/Mask • flush with water contact.
U028 • Imperious gloves • very corrosive
• Chemical resistant
suit/boot
P124 Solvents • Lab coat (anti-fire) • soak with sand a • flammable, P124 • most aromatic compounds are
• Glasses • avoid any ignition FP=46F,AFT=995F Carcinogenic.
U101 • Gloves • go flammable container • Water fog, alcohol foam, • easy to evapor to cause fire
• Solvent-resistant (steel) CO2 or Dry chemicals. • operating in exaust-hood
Mask/respirator • FP/AFT increase with MW of
homologous compounds
U051 Petro-fractions • Lab coat (anti-fire) • soak with sand a • flammable U051 • Carcinogenic.
• Glasses • avoid any ignition FP=135F,AFT=475F • easy to evapor to cause fire
• Gloves • go flammable container • Water fog, alcohol foam, • operating in exaust-hood
U052 (plastic) CO2 or Dry chemicals. • FP/AFT increase with MW of
homologous compounds
J218 oxidizers • Clean clothing • Scoop to container a • deluge with water • J496 powderous to cause cause
• Goggles • Flush water • support firing. respiratory problem
• Gloves • All oxidizers support firing
• Dust-free mask
163

MEA CSL Stimulation Laboratory Procedures

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MEA CSL Stimulation Laboratory Procedures

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SCHLUMBERGER MEA TECHNOLOGY HUBMEA STIMULATION CLIENT SUPPORT

MEA CLIENT SUPPORT LABORATORY

July 15, 2002

MASTER TABLE OF CONTENTS

SECTION 1 HYDRAULIC FRACTURING

SECTION 2 MATRIX ACIDIZING

SECTION 3 FOR MATION DAMAGE

SECTION 4 CORE ANALYSIS

SECTION 5 SAND CONTROL AND WATER CONTROL

SECTION 6 ANALYTICAL METHOD

SECTION 7 LABORATORY SAFETY

SECTION 1 HYDRAULIC FRACTURING

HF-001 ClearFRAC Laboratory Preparation

• Pour 500ml of water into the blender jar and stir.

HF-002 YF100HTD Laboratory Preparation

Equipment and Materials

Waring blender equipped with variable transformer

Linear Gel Preparation

HF-003 YF800HT Laboratory Preparation

Equipment and Materials

Waring blender equipped with variable transformer

Additives in a typical YF845HT system

Linear Gel Preparation

Gel Crosslinking(recommend using microwave)

HF-004 YFGO”III” Laboratory Preparation

• Mixing of Activator Solution

YFGOIII is prepared by simultaneously adding J452 Gelling Agent and activator

• Mix at 10,000 rpm for 10 minutes.

HF-005 YF100LG Laboratory Preparation

--- Slowly add 2.55g of J494 to the vortex.

--- Slowly add 1.06g of M3 to the vortex.

HF-006 YF100LGD Laboratory Preparation

with 1gal/1000 J450 = 7.8 gal/1000gal (or 1.56mL/200mL)

Desired concentration Equivalent to gal of 30% Equivalent to mL of 30%

--- Inject the delay agent and blend for 2 minutes.

HF-007 PrimeFRAC Laboratory Preparation

Equipment and Materials

Waring blender equipped with variable transformer

Linear Gel Preparation

Gel Crosslinking and Delaying

Conductivity and Specific Gravity for J513 Standard Solutions

Typical J513 Standard Curve

HF-008 SXE Laboratory Preparation

HF-009 Fann35 Linear Gel Viscosity Measurement

The fluid viscosity can be determined by the following equation

F0.2 0.2 0.9 333.3 R1-B1 1.000

Chan35 - Linear Gel Viscosity Test

HF-010 Static Gel Break Test

1000ml jar with cap

• Prepare the base gel as described in different fluid preparation procedures.

Test Procedures (for temperature greater than 100C, qualitative method)

HF-011 HTHP Gel Rheology Test (Fann50 Model Viscometer Operation)

• Power on the machine and computer until NORDDAQ program manager.

The floowing equations are used in the instrument for calculation

NI Rheometer – HTHP Fracturing Fluid Rheology Test

HF-012 Fracturing Sand Sieve Analysis (API RP56/60)

Recognized Fracturing Sand Sizes

Recognized High Strength Proppant Sizes

Sieve opening sizes 1700/850 1180/850 850/425 425/212

ASTM Standard Sieves and Endecotts Sieve Shaker

HF-013 Proppant Sphericity and Roundness (API RP56/60)

Particle sphericity is a measurement of how closely a sand particle or grain

Equipemnt and Materials