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JET Manual 38
WPS-Basic
Laboratory Training
and Fluid QA/QC
Version 1.0
JET Manual 38 WPS-Basic Laboratory Training and Fluid QA/QC
InTouch Content ID# 4298920
Version: 1.0
Release Date: June 05, 2007
Owner: Well Services Training & Development, IPC
Schlumberger private
Document Control
Revision History
Rev Effective Date Description Prepared by
Copyright © 2007 Schlumberger, Unpublished work. All rights reserved.

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Other company, product, and service names are the properties of their respective owners.
Table of Contents
1.0 Introduction 5
1.1 Learning objectives 5
2.0 Safety Considerations 7
2.1 Personal protective equipment (PPE) 7
2.2 Emergency equipment 7
2.3 Chemical spills 8
2.4 Key Service Quality Requirements (KSQR) 8
3.0 Laboratory Truck and Technician 11
4.0 QA on Location 13
4.1 Water tests 13
4.1.1 Iron concentration test 13
4.1.2 Bicarbonate concentration 14
4.2 Gel tests 14
4.3 Other QA tasks while pumping 15
5.0 Typical Laboratory Tests 17
5.1 Water analysis 17
5.1.1 pH, specific gravity, and turbidity 17
5.1.2 Alkalinity (indicator method) 20
5.1.3 Chloride 21
5.1.4 Calcium and magnesium 21
5.1.5 Sulphate, barium, iron, and potassium 23
5.1.6 Sodium (calculation method) 24
5.2 Linear fluid viscosity 25
5.2.1 Water-base fluid linear gel viscosity 25
5.3 Vortex closure 26
5.4 Fracturing fluid crosslink delay 27
5.5 Static gel break test 28
5.6 HPHT gel rheology 30
5.7 Fracturing sand sieve analysis 31
5.7.1 Sampling techniques 32
5.7.2 Sand sieve analysis (modified API method) 32
5.8 Proppant turbidity test 33
5.9 Silt turbidity test 34
JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | iii

5.10 Proppant sphericity and roundness 34
5.11 Fluid compatibility with RCP 35
5.12 Vapor pressure test 36
6.0 Hydraulic Fracturing Fluids 37
6.1 Linear gel 37
6.2 YF1xxHTD fluids 38
6.3 YF8xxHT fluids 40
6.4 YF”GO”-III fluid 41
6.5 YF100LG fluids 42
6.6 YF100LGD fluid 44
6.7 Crosslink delay 45
6.8 PrimeFRAC fluids 45
6.8.1 Crosslinking and delay times 46
6.8.2 RCP/PrimeFRAC compatibility 47
6.8.3 QA/QC for J464L, J494L, and J513 47
6.9 Super X emulsion 49
6.10 ClearFRAC J508W 50
7.0 Matrix Acidizing Fluids 51
7.1 HCl 51
7.2 Intensified Acid 52
7.3 Clay acid 52
7.4 Mud acid 53
7.5 Organic mud acid 55
7.6 Organic clay acid 56
7.7 Alcoholic acid 56
7.8 Dynamic acid dispersion (DAD) 57
8.0 QA/QC Practices 59
8.1 Fracture fluid QA/QC 59
8.2 Fracture fluid additives QA/QC 60
8.2.1 J515 62
8.2.2 LGD Crosslinker 62
8.2.3 U028 63
9.0 References 65
10.0 Check Your Understanding 67
iv | Copyright
1.0 Introduction
The fracturing fluid is a critical component of

the hydraulic fracturing treatment. Its main
functions are to open the fracture and to
transport propping agent along the length of
the fracture. To make sure that the fluid and
proppant pumped is of the best quality and to
maintain the quality during the treatment, the
laboratory technician must perform a variety of
tests. This module introduces basic field and
laboratory tests that employees performing the
fluid tests should know.
1.1 Learning objectives

The objective of this manual is to introduce you
to Well Productivity Services (WPS) basic lab
training and fluid QA/QC. After reading this
manual, you should be able to do the following:
• Perform water analyses.

• Understand Fann® Model 35 viscometer
operation and perform gel viscosity
measurement.
• Understand the vortex closure test.
• Perform the fracturing fluid crosslink delay
test.
• Perform the static gel break test.
• Understand Fann Model 50-type
viscometer operation and perform an
HPHT gel rheology test.
• Perform sand sieve analysis.
• Prepare hydraulic fracturing fluids.
• Prepare matrix acidizing fluids.
• Understand fracturing fluids QA/QC.
JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 5

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6 | Introduction
2.0 Safety Considerations
All employees working in fracturing laboratory ○ Rubber or plastic protective aprons

must follow specific rules and procedures to must be worn, depending on the type
prevent injuries and loss of equipment. of chemical. Read the MSDS for each
chemical for the protective clothing
All Well Services (WS) and Oilfield Services requirements.
(OFS) safety standards must be complied with.
○ Types of clothing that allow exposure to
All personnel should review Well Services
a large area of skin must not be worn in
Standard 24, Laboratory Operation, InTouch
a laboratory (e.g., sleeveless tops, short
Content ID# 3313702.
skirts, or short pants).
• other requirements
2.1 Personal protective equipment (PPE)
○ Safety boots are not required in
Proper personal protective equipment (PPE) the laboratory. Shoes that provide
should be worn while working in the laboratory. protection from liquids must be worn,
such as a leather shoe that covers the
• eye protection foot. Sandals and open shoes are not
○ Safety glasses with fixed side shields permitted.
are required at all times as minimum ○ Gloves must be worn when handling
eye protection (this requirement does chemicals, according to the MSDS.
not apply to offices, restrooms, or other
protected areas not in the laboratory Please refer to SLB QHSE Standard S003,
working area). Personal Protective Equipment, InTouch
Content ID# 3260259, for more information.
○ Indirect vented chemical goggles must
be worn when handling chemicals such
as cement, unless these chemicals are 2.2 Emergency equipment
in sealed containers. The following lists the emergency equipment
○ Face shields must be worn when that must be available.
handling hot liquids, acids, or liquids
that are under pressure, or working with • Every WS laboratory must have at least
flammable liquids where the flash point is one eyewash station and one emergency
less than 100 degF. shower.
○ Visitors must wear safety glasses with • Fire extinguishers must be easily
side shields while in the laboratory work accessible in case of fire.
areas. • Every laboratory must have a complete first
• protective clothing aid kit.
○ Laboratory coats with long sleeves must • Fire blankets must be available in any
be worn as the minimum protective laboratory where tests are performed with
clothing. flammable liquids.

• Chemical spill control kits are necessary for • Chemicals must not be put into a sink drain
the laboratory. The kits must include rubber or any drain that is connected to a sewer or
gloves, absorbent material or spill booms, waste water drainage system.
disposal bags or containers with labels,
• All drain pipes must comply with local
and a mercury spill control kit, if mercury is
regulations. The contents of all drains must
used in the laboratory.
be analyzed every 12 months. The data
• Laboratories must have easy access must be recorded and kept on file.
to exits so that personnel can leave the
• Please refer to WS Safety Standard 24,
laboratory in case of a fire.
Section 11.2, for instructions for mercury
• Emergency numbers and procedures spills.
must be displayed at the entrance to the
laboratory. 2.4 Key Service Quality Requirements
(KSQR)
2.3 Chemical spills
It is crucial to follow the Fracturing Key Service
The following lists the precautions that must be Quality Requirements (InTouch Content ID#
taken for chemical spills. 4147789) for successful job preparation and
execution.
• Each laboratory and laboratory field van
must be equipped with the spill disposal kit. The following points specify the laboratory
• A spill response plan should be prepared operations:
that follows this general outline:
Design and preparation requirements
a. Make sure all personnel are
removed from the area. • Follow proper lab procedures.
Responsible: LM
b. If flammable or combustible fluids
are used, shut off or remove all • Perform base fluid lab testing on any of
possible sources of ignition. the following applications: jobs above
82 degC [180 degF]; new client; new
c. Stop the chemical discharge. formation; new technology or new product.
Testing to include breaker testing (schedule
d. Apply absorbent material to control generation and verification) completed prior
all free liquids and place any mate- to job at bottomhole temperature and Fann
rial into a disposal container found 50 for cross-linked fluids. Responsible: LM
in the spill disposal kit. • Verify chemical load out volumes and
additive calculations before loading the job.
e. Add a label to the disposal container Responsible: LM, JS
that shows the contents and date.
• Follow documented loading and sampling
f. Place the container with other procedures for the fracturing fluid systems
chemicals ready for disposal. being used. Responsible: LM, JS
• Reverify chemical volumes and additive
g. Report the spill to the health, calculations before transporting to the
safety, and environment (HSE) wellsite or wellsite storage. Responsible:
representative. LM, JS
8 | Safety Considerations
• Line management conducts with the JS
a job brief/review/discussion that includes
discussion/completion of:
○ SQ risk assessment
○ job design and procedure
○ job sheet with relevant well information.
Responsible: LM
• Wellsite execution requirements

• Crew has and uses proper and functional
personal protective equipment (PPE).
Responsible: JS
• Conduct prejob meeting with client
representative, crew, and involved third
parties to agree on job procedure,
design, calculations and Service Quality
contingency plans. Responsible: JS
• Rig up in compliance with QHSE
standards. Responsible: JS
• Record critical job parameters (density,
rate, pressure/s, liquid additives).
Responsible: JS
• Perform mass balance requirements.
Responsible: JS
• Perform sample requirements and onsite
fluid QA/QC requirements. Responsible: JS
• Pump the job as designed. Any deviation
from original job procedure requires
agreement with client representatives.
Responsible: JS and LM.

10 | Safety Considerations
3.0 Laboratory Truck and Technician
A laboratory truck (Fig. 3-1) or similar dedicated laboratory unit, equipped with basic fluid quality
testing tools (Fig. 3-2) must be present at the job site during a fracture treatment.
Figure 3-1. Field Laboratory Truck
Mud balance Digital titrator
Water bath Retort kit

Balance
Field QA/QC kit

Production
screen tester Hydrometers
Graduated cylinders
Syringes
Flasks
Beakers
Sample bottles
Reagents Stopwatch
Process
controlled
rheometer
Bacteria Conductivity meter Emulsion Variable
luminometer Remote laser thermometer stability speed
Dry probe pH meter meter mixer
Figure 3-2. Field QA/QC Kit

Fluid samples gathered from the field blending
equipment, or fracture tanks if batch mixed,
are checked for quality control. On land-
based fracture treatments, the fluid is most
often mixed in a PCM* precision continuous
mixer and supplied to a POD* programmable
optimum density blender. The quality assurance
(QA) that can be performed with this truck
in the field lab ensures that the treatment is
executed as designed. Simple QA steps can
greatly increase the odds of success for a
hydraulic fracturing treatment.
The laboratory technician (Fig. 3-3)
• works under the direction of the job

supervisor to collect samples and perform
fluid quality control
• must understand the principles of
stimulation and fluid rheology
• must be able to calculate and prepare
solution concentrations and additives
• checks the quality of the water before gel is
prepared
• collects samples for testing and
troubleshoots all problems of hydration, gel
loading or crosslinking.
Figure 3-3. Laboratory Technician Hard at Work
12 | Laboratory Truck and Technician

4.0 QA on Location
The following are QA tasks that will need to

be performed on location before pumping the
STEP 03 Insert the tube of prepared
sample into the right top opening of the
stimulation treatment.
comparator.
4.1 Water tests STEP 04 Fill the other color viewing tube
with an untreated water sample. Place it in the
Tests must be performed on the mix water for
left top opening of the color comparator.
• temperature
• pH
STEP 05 Hold the comparator up to a light
source and view through the openings in front.
• specific gravity–hydrometer method Rotate the disc to obtain a color match. Read
the mg/L iron (Fe) concentration through the
• iron concentration
scale window.
• bicarbonate concentration.
You will need a sample of water from each STEP 06 If the concentration is greater than
tank (3 to 5 L). At least 1 L of water should be 10 mg/L, perform another test with a diluted
reserved in case additional testing is necessary sample as follows:
in the district laboratory after the fracture, such
as in the case of a screenout. 1. Use a 1-mL sample of water to be
tested and 4 mL of distilled water.
Test the water parameters to ensure that they
are within the range of acceptable values for 2. Follow the procedure in Steps 1 through
the fluid pumped. 5, but multiply the results by 5.
4.1.1 Iron concentration test

Perform this test as follows, using a HACH iron
test kit:
STEP 01 Insert the iron color disk into the

comparator.
STEP 02 Fill a clean color test tube to the

5-mL mark and then add the chemical packet to
the tube and shake to mix. An orange color will
develop if iron is present.

4.1.2 Bicarbonate concentration with the PCM or GelSTREAK and perform the
following tests.
Follow this procedure to test for bicarbonate
concentrations.
STEP 01 Measure the pH of the linear gel
and record.
STEP 01 Measure 100 mL of undiluted
sample into a 300-mL glass beaker.
STEP 02 Divide the linear gel into 2
beakers of 250 mL each.
STEP 02 Insert a clean delivery tube into
the titration cartridge (1.6N H2S04). Attach the
cartridge to the titrator body. STEP 03 Make a crosslinked solution using
volumes recommended in laboratory testing.
STEP 03 Hold the digital titrator with the
cartridge tip pointing down. Turn the delivery STEP 04 Start the mixer at a low speed and
knob to eject air and a few drops of titrant. add the chemicals.
STEP 04 Reset the counter to zero and STEP 05 Measure and record the time it
wipe the tip. takes for the fluid to have a vortex closure in the
mixer and the time it takes for the fluid to have
a good hang lip (crosslink).
STEP 05 Add the contents of one
Bromocerol green-methyl red indicator powder
packet to the glass beaker and swirl to mix. STEP 06 Test and record the pH of the
crosslinked fluid.
STEP 06 Titrate with sulfuric acid to a
light pink color. As the titration progresses, the STEP 07 Borate fluid systems only: Perform
colors will change from light greenish blue-gray a shear test of the fluid by submitting it to high
to light pink. speeds in the mixer and ensuring that the fluid
will heal itself after shear.
STEP 07 Record the value shown on the
digital titrator as the total bicarbonate (the units STEP 08 Perform a breaker test
are in mg/L as CaCO3). at bottomhole temperature (BHT). Use
concentrations dictated by the latest laboratory
report to add the correct amount of breaker to a
4.2 Gel tests beaker of crosslinked gel. Place the sample into
The linear gel must be tested before beginning a water bath at bottomhole temperature. Test
the job. A linear gel sample prepared with and record the time until the gel starts to break.
the actual water and chemical samples on
location must be mixed and analyzed before
job fluid mixing commences. Use the procedure
detailed in Section 6-1, check the viscosity of
the gel using the Fann 35-type viscometer and
compare the tested viscosity and temperature
with the expected ranges. When this sample
meets the specification, begin initial mixing
14 | QA on Location
4.3 Other QA tasks while pumping
The following are common QA tasks while
pumping:
• Throughout the job, linear gel should

be continually checked for viscosity and
temperature to confirm the proper gel
loading.
• Samples should be taken from the outlet
of the blender or fracture pumps to test
the delay time of the crosslinked fluid as
well as pH, temperature, BHT stability, and
break testing (water bath).
• The physical quantities of all liquid and dry
additives should be continually checked
throughout the job to compare to the
designed amount to be pumped.

16 | QA on Location
5.0 Typical Laboratory Tests
Several tests are commonly performed at the 5.1.1.1 pH

district laboratory before the job.
The normal pH range for brines is between
6 to 8. A low pH may indicate spent acid,
5.1 Water analysis whereas a high pH may indicate contamination
by mud or filtrate. Some of the constituents
The oil industry uses water analysis for quality that control the pH of water are dissolved
control, formation identification, compatibility solids, precipitation of iron, carbon dioxide,
studies, and environmental evaluations. bicarbonate, borate, and hydrogen sulfide. The
pH of water can strongly affect the hydration
The following procedures have been developed
of a polymer and mechanism of some cross-
to perform the necessary water analyses.
linking reactions. It should be tested using pH
paper and a digital pH monitor.
• pH testing (meter)
• specific gravity testing (hydrometer and SG The pH paper is appropriate for a quick check
bottle method) on most fluids, providing the paper is not old
and has not been exposed to extreme heat or
• turbidity testing (HACH method)
sunlight. The pH paper test procedure is very
simple:
5.1.1 pH, specific gravity, and turbidity
The following describes how to test water for STEP 01 Dip a piece of pH paper into the
pH, specific gravity, and turbidity. water sample.
You will need the following items:
STEP 02 Match the color of the paper with
• pH meter and calibration fluids the chart on the package of pH paper.
• SG bottle For a more accurate reading, a pH meter

should be used:
• balance
• filtering apparatus and accessories (filter
paper, vacuum pump and funnel assembly)
STEP 01 Calibrate pH meter as described
in the pH meter manual.
• deionized (DI) water
• water sample STEP 02 Shake the water sample to
homogenize it.
Filter the sample if not clear by observation.
Save the filtrate for further analysis.
STEP 03 Insert the pH probe into the water
Follow the procedures in the following sections sample.
to test the water.

STEP 04 Read the pH after the reading STEP 03 Read the value for specific gravity
stabilizes on the meter screen. Check the where the top of the fluid intersects one of the
temperature. Record the pH and temperature. lines on the hydrometer.
Note:
STEP 04 The value for specific gravity
should be corrected for temperature by using
• The closer the pH is to 8.0, the the temperature correction table (rule of thumb:
slower the gel will hydrate. Add 0.0002 to the SG for every degree above
60 deg).
• If the pH is close to or equal to
8.0, it is recommended to buffer HCl strength can also be determined from its
with acid. specific gravity and compared to the chart in
the acid strength chart found in the Field Data
• If the pH is above 8.0, the water Handbook.
must be buffered.
Use this equation to relate API gravity to
• If buffering the tank, add
specific gravity:
1 galUS 36% HCl per
20,000 galUS and check the
141.5
pH. If the pH is at or above 7.5, SG=
131.5 + API
add HCl by the quart until the
pH is below 7.5.
141.5 – 131.5(SG)
API=
SG
5.1.1.2 Specific gravity

Specific gravity is the ratio of the weight of
material to the weight of water, or the density of Note:
the material to the density of water. Fresh water The higher the API gravity is, the
has a specific gravity of 1.000. The higher the lighter the fluid is.
specific gravity is, the heavier the liquid will be.
Specific gravity can be used to differentiate
hydrocarbons (condensate) from water. A
SG Bottle Procedure:
hydrometer is used to measure specific gravity.
Follow this procedure to determine the SG
Hydrometer procedure (the preferred using the SG bottle.
method in the field):
STEP 01 Fill a graduated cylinder with the

STEP 01 Weigh the empty SG bottle and
record the weight as W1.
fluid to be tested. Use a 100-ml cylinder for a
7-in hydrometer and 250-ml cylinder for a 12-in
hydrometer. STEP 02 Fill the bottle with DI water until
water runs out of the capillary and cap it.
STEP 02 Carefully drop the hydrometer into
the liquid with a slight spin.
18 | Typical Laboratory Tests

STEP 03 Weigh the bottle containing DI STEP 03 Fill a clean sample cell with 25 mL
water and record the weight as W2. of the water sample and another clean sample
cell with 25 mL of DI water.
STEP 04 Clean the bottle to be used for the
water sample three times, fill it with the water STEP 04 Insert the DI water sample cell
sample, and cap it. into the cell holder and close the shield.
STEP 05 Weigh the bottle containing the STEP 05 Press ZERO to zero the machine.
water sample and record the weight as W3.
STEP 06 Place the sample cell with the
STEP 06 Clean everything you used for this sample water into the holder and close the
test with DI water. shield.
To calculate the SG of the sample water, use

this formula:
STEP 07 Press READ/ENTER to obtain the
FTU water turbidity.
(W3 – W1)
SG=
(W2 – W1) STEP 08 Turn off the HACH2000 and clean
up the cells with DI water.
5.1.1.3 Turbidity
Make sure to use unfiltered water for this test.
STEP 01 Switch on the HACH2000

spectrophotometer (Fig. 5-1) and enter the
method #750.
Figure 5-1. HACH2000 Spectrophotometer
STEP 02 Adjust the wavelength to 450 nm

for the test.

5.1.2 Alkalinity (indicator method) If the sample did turn pink, continue to Step 05.
Fluids should be tested for alkalinity.
Bicarbonates, carbonates, and hydroxide can STEP 02 If the sample did not turn pink add
all increase the alkalinity. ½ dropper methyl purple.
Bicarbonates are very important for fracture STEP 03 Titrate with 0.1N HCl or 0.0164 N
fluid quality control. Fracturing fluids require HCl to the purple endpoint.
various bicarbonate concentrations depending
on the specific fluid. High bicarbonate
concentrations will tend to slow gel hydration
STEP 04 Calculate the bicarbonates
concentration:
and delay fluid crosslink. If high bicarbonate
concentrations are encountered, the fluid may • For 0.1N HCl, bicarbonates (mg/L)
be treated with calcium chloride (S1), which = mL of 0.1N HCl x 122
will create calcium and bicarbonate bonding.
The calcium bicarbonate will precipitate, • for 0.0164N HCl, bicarbonates (mg/L)
thereby reducing the dissolved bicarbonate = mL of 0.0164N HCl x 20
concentration. The precipitate will not interfere
with the fluid. Note:
These equations are valid only for
The other reason to determine the bicarbonate
50-mL samples.
concentration is to identify the water source.
High bicarbonate concentrations may be
characterized by a high pH or be an indication
of carbonates present in the water. STEP 05 If the sample did turn pink after
Step 01, titrate with 0.1 N HCl until the pink
Most formations do not contain carbonates color disappears. The amount of 0.1N HCl used
or hydroxides. If a water sample contains will be P in the calculations.
carbonates and/or hydroxide, it may be a clue
to a problem in the customer’s well, possibly STEP 06 Add 3 drops of methyl purple.
indicating the presence of some drilling mud
contamination.
STEP 07 If sample turns green, titrate with
Most oilfield waters contain only bicarbonates, 0.1 N HCl to the purple endpoint. The total
but occasionally carbonate and/or hydroxide will amount of 0.1 N HCl used in both titrations will
be present. be T in the calculations.
Follow this procedure to test the alkalinity. Use STEP 08 Perform the calculations indicated
a 50-mL sample regardless of the specific in Table 5-1.
gravity.
Table 5-1. Alkalinity Indicators
STEP 01 Add 3 drops of phenolphthalein

Indicator Bicarbonates Carbonates Hydroxides
indicator. P<1/2T T-2P 2P None

P=1/2T None 2P None
If the sample did not turn pink, the sample does P>1/2P None 2(T-P) 2P-T
not contain carbonates or hydroxide. Continue P=T None None T
with Step 02.

where STEP 04 Titrate to the orange/red endpoint
with 0.1N silver nitrate.
• P = amount of 0.1 N HCl required to titrate
sample to a colorless endpoint after adding
phenolphthalein
Note:
• T = amount of 0.1 N HCl required to titrate If a sample contains H2S (it will
sample to colorless endpoint after adding have a rotten egg smell), heat the
phenolphthalein plus the amount of 0.1 N sample until the odor is eliminated.
HCl required to titrate sample to the purple
endpoint after adding of methyl purple.
• bicarbonate (mg/L) = (mL of 0.1N HCl) (122) STEP 05 Perform the following calculation:
• carbonates (mg/L) = (mL of 0.1N HCl) (60)
(3545)(mL of silver nitrate)
• hydroxides (mg/L) = (mL of 0.1N HCl) (34). Cl(mg/L)=
sample size (mL)
5.1.3 Chloride
For concentrations of silver nitrate other than
Most fracture fluids today contain 2% KCl. The
0.1N, use this calculation:
chloride content of a 2% potassium chloride
solution should be approximately 9,600 mg/L.
Cl(mg/L)=
The chloride test can also be used to determine (mL of silver nitrate)(normality of silver nitrate)(35,500)
if a sample is spent acid. The characteristics of sample size
spent acid are a high chloride content and a pH
of approximately 3.0 to 6.0.
5.1.4 Calcium and magnesium

STEP 01 Check SG to determine proper
sample size according to Table 5-2. The following sections describe how to
determine the calcium and magnesium content
Table 5-2. SG of Fluid vs. Amount of Sample in the water. Magnesium and calcium are the
most common sources of hardness in produced
Specific Gravity Amount of Sample
waters; any other components that may
1.000 to 1.003 50 mL contribute to total hardness are negligible.
1.003 to 1.020 10 mL
1.020 and over 1 mL
STEP 02 Dilute to 50 mL with distilled

water.
STEP 03 Add 3 to 4 drops of potassium

chromate.

5.1.4.1 Calcium (mL EDTA used)(molarity of EDTA)(40,100)
Ca(mg/L)= sample size
Most produced water will have less
than 15,000 mg/L of calcium. If higher
concentrations of calcium are encountered,
the water is almost certainly from a limestone
or dolomite formation that has recently been 5.1.4.2 Magnesium
acidized. If less than 15,000 mg/ L calcium is The magnesium test used (standard titration
detected, continue the water analysis. method) is a test for total hardness. This
test assumes that the water hardness is due
Follow this procedure to determine the calcium to dissolved magnesium and calcium only.
content. Generally, the magnesium concentration is
used for total dissolved solids calculations
STEP 01 Determine the correct sample to identify the water source. However, high
size. The sample size depends on the SG of magnesium is generally due to a recent acid
the fluid; see Table 5-3. treatment of a dolomite formation.
Table 5-3. Amount of Sample vs. Specific Gravity The following standard titration method
requires that calcium be determined before
Specific Gravity Amount of Sample
the calculating the magnesium concentration.
1.000 to 1.003 50 mL Subtract the calcium concentration from the
total hardness and assume the remaining
1.003 to 1.020 10 mL hardness is due to magnesium.
1.020 and over 1 mL
Follow this procedure:
STEP 02 Dilute the sample (if less than STEP 01 Determine correct sample size.
50 mL) to 50 mL with distilled water.
STEP 02 Dilute to 50 mL with distilled
STEP 03 Add 3 to 4 drops NH4OH. water.
STEP 04 Add 2 scoops of Calver II STEP 03 Add 3 to 4 drops NH4OH.

hardness reagent.
STEP 04 Add 2 scoops of Univer II
STEP 05 Titrate with 0.025 M EDTA to the hardness reagent.
blue endpoint.
STEP 05 Titrate with 0.025 M EDTA to the
STEP 06 Perform the following calculations: blue endpoint.
(mL of 0.025 MEDTA used)(1,000)
Ca(mg/L)=
sample size
For EDTA concentrations other than 0.025 M,

use this equation:

Follow these procedures.
Note:
This test is for the total hardness. STEP 01 Switch on the HACH2000.
To find the amount of 0.025 M
EDTA for magnesium, subtract the Repeat Steps 02 through 14 for each
number of mL of 0.025 M EDTA contaminant being tested for.
used to determine calcium. This
difference is the number of mL of
0.025 M EDTA used to determine
STEP 02 Enter the appropriate stored
program number (680 for sulphate, 20 for
the magnesium.
barium, 265 for iron, and 950 for potassium).
STEP 06 Perform the following calculation: STEP 03

Rotate the wavelength dial
until the display shows 450 nm for sulphate
Mg(mg/L)= or barium, 510 nm for iron, or 650 nm for
[(mL of 0.025 MEDTA for Mg) – (mL of EDTA for CA)](606) potassium.
sample size
STEP 04 Press READ/ENTER.
For EDTA other than 0.025 M, calculate STEP 05 Pour 25 mL of sample into the
sample cell.
Mg(mg/L)=
[(mL of 0.025 MEDTA for Mg) – (mL of EDTA for CA)](molarity EDTA)(24,340)
sample size STEP 06 Add the contents of appropriate
reagent powder pillow to the sample cell (the
prepared sample). Swirl to dissolve.
5.1.5 Sulphate, barium, iron, and STEP 07 Press SHIFT TIMER.

potassium
To test the quantity of sulphate, barium, STEP 08 When the timer beeps, fill another
iron, and potassium in the sample using the sample cell (blank) to 25 mL of sample. Place it
HACH2000 spectrophotometer, you will need into the cell holder and close the light shield.
the following items:
STEP 09 Press ZERO to zero the machine.
• HACH2000 with accessories
• DI water STEP 10 Within a few minutes after the
• SulfaVer® Reagent Powder Pillow for
timer beeps, place the prepared sample into the
SO42- cell holder. Close the light shield.
• BariVer® 4 Reagent Powder Pillow for

Ba2+
STEP 11 Press READ/ENTER.
• FeroVer® Iron Reagent Powder Pillow, for STEP 12 Record the reading.
Fe2+/Fe3+
• potassium I/II/III reagent, for K+
• water sample.

STEP 13 Dilute the sample if the reading fills the ampoule and begins to mix with the
reagent.
flashes (over limit) and repeat the above
procedures.
Note:
To determine the quantity of the contaminant,
A small bubble of inert gas will
use the following equation.
remain in the ampoule to facilitate
• contaminant content (mg/L) = HACH2000 mixing.
reading × dilution factor (if any)
5.1.5.1 Iron (HACH method) STEP 05 Remove the VACUette from the
dilutor snapper cup. Mix the contents of the
When high iron is encountered in fracture fluid VACUette by inverting it several times, allowing
mix water, breaker J218 (ammonium persulfate) the bubble to travel from end to end each time.
will have an accelerated effect. In high iron
environments, J218 may cause premature
breaking of the fracture fluid.
STEP 06 After 1 min, use the appropriate
comparator to determine the level of iron in the
sample.
In addition, high iron content will interfere with
the crosslinking of the fracture fluid, resulting in
poor crosslink integrity. 5.1.6 Sodium (calculation method)
To determine the sodium content of the water
The maximum iron concentration for fracturing
using the results of the tests described in
water ranges from 8 to 25 ppm, depending on
Sections 5.1.1 through 5.1.5, use this equation:
the fluid.
• mg/L of Na+
You will need a CHEMetrics kit.
= 23 × (A/35.5 + B/61 + C/60 + D/17
Follow this procedure to determine the iron – E/56 – F/137 – G/24 – H/40 –I/39)
content. where
• A = chloride (mg/L)
STEP 01 Fill the dilutor snapper cup to the
25 mL mark with iron-free water. • B = bicarbonate (mg/L)
• C = mg/L of carbonate (mg/L)
STEP 02 Fill the microtest tube halfway with
• D = mg/L of OH- (mg/L)
your sample.
• E = mg/L of iron (mg/L)
STEP 03 Holding the VACUette almost • F = mg/L of barium (mg/L)
horizontally, touch the tip to the contents of
the micro test tube. The tip fills completely by • G = mg/L of Mg2+ (mg/L)
capillary action. • H = mg/L of Ca2+ (mg/L)
• I = mg/L of K+ (mg/L).
STEP 04 Completely immerse the
VACUette tip into the contents of the dilutor
snapper cup. Snap the tip of the ampule and
wait until the VACUette fills up. The sample

5.2 Linear fluid viscosity • water sample.
To determine the viscosity of linear fluids (in- The approach is to hydrate the polymer
cluding water-based fracturing fluids, gelled oils, following the Fracturing Materials Manual
and gelled acids), the Fann® Model 35 rheom- (InTouch Content ID# 4223817) procedures,
eter (Fann 35) is primarily used. sample the fluid, load the fluid into the Model
35 sample cup, and record the bob deflection
Follow these practices to calibrate the at different rotor rotational speeds. Generally
rheometer: six rpms are available: 3, 6, 100, 200, 300,
600 rpm.
• Perform a full calibration Monday of each
week or each 75 hours of operation, STEP 01 Power on the Fann 35.
whichever comes first.
• The rheometer must be cool and clean. STEP 02 Install the rotor and bob if they are
• The rheometer must agree with the not in there already.
calibration oil chart to within ±1 cP.
• If the rheometer does not calibrate, then
STEP 03 Fill the sample cup to the mark
with fracturing fluid.
service the unit or send out for repair as
instructed by the instrument manual.
• After each test, do the following:
STEP 04 Place the sample cup on the
stage. The three pins on the bottom of the cup
○ Take off rotor and bob. Clean each piece sit in three holes on the stage.
with soap and water.
○ Wipe off the shaft with a damp cloth in STEP 05 Raise the stage until the sample
a down motion. Do not press against cup is at the mark on the rotor.
the shaft-up motion pushes fluid up the
shaft. STEP 06 Set the Fann 35 to the desired
○ Reassemble unit ensuring that each shear rate.
piece is finger-tight. Tightening the bob
or the rotor too much can damage the
shaft and torque transducer.
Note:
Shift gears only when the
instrument is running.
5.2.1 Water-base fluid linear gel viscosity
• Fann 35 viscometer with appropriate STEP 07 Let the dial come to a steady
parameters (speed factor, R-B factor and reading and record the reading.
spring factor)
• rotor and bob
STEP 08 Measure and record the fluid
temperature.
• Fann 35 sample cup
• fracturing fluid
• thermometer

STEP 09 Compare the reading with the crosslinking has occurred and an elastic
lipping material has formed.
appropriate hydration curve. All laboratories
and laboratory trucks should have the hydration
curves onsite; you can also find them in the It is important to determine the time to both
Fracturing Materials Manual, InTouch Content vortex closure and fluid crowning during a
ID# 4223817. vortex closure test.
• Allow gel to hydrate for an additional 10 min

if the viscosity is 95% of the nominal value. Note:
Continuing to shear the fluid after
• Verify the pH and water temperature are
vortex closure will degrade the
within the prescribed limits.
thermal stability and appearance
• Add polymer in 2-ppt increments if the of the gel. Therefore, you must
viscosity is still low after 10 additional prepare a new fluid sample for
minutes of hydration and the pH and water breaker tests or for baseline fluid
temperature are within specifications. performance characterization; do
not use the same fluid sample
5.3 Vortex closure from which the vortex closure and
crowning times are determined.
Vortex closure is one method for estimating
a crosslink time, as are the crosslink delay
temperature and crosslink delay time tests.
To perform this test, you will need the following
But, whereas the crosslink delay temperature
items:
or crosslink delay time tests indicate the time
or temperature required to achieve a lipping
• Waring blender
fluid, the vortex closure test simply indicates
the onset of viscosity development (and rarely • timer
coincides with full crosslinking). • fluid to be tested, including all additives
There are three distinct fluid behaviors during a • crosslinker to be tested.
vortex closure test: Follow these procedures to perform the vortex
closure test.
1. The first is the linear fluid behavior.
This is the initial state of the fluid and is
characterized by a deep vortex. STEP 01 Prepare 250 mL of the base fluid
(KCl or L64, surfactants, stabilizers, and buffers
2. The second is the viscosity increase for polymer fluids; the fracturing oil and the
that results in vortex closure, but does recommended additives for gelled oils). Include
not stop fluid circulation in the blender all additives except the crosslinker.
cup.
STEP 02 Add the base fluid to a 1-L glass
3. The third behavior is fluid crowning, Waring blender cup. Adjust the mixing speed to
which is the formation of a dome of develop a deep vortex. The top of the blade nut
fluid over the center of the blender cup should just be visible, but the flats of the blade
(over the blades). This is the point at should not be covered in the fluid.
which the fluid no longer completely
circulates in the blender cup. It indicates

STEP 03 Simultaneously add the Note:
crosslinker/activator package and start a timer.
Most temperature-activated
fluids will still crosslink at low
STEP 04 Record the time at which the temperatures after some time.
vortex closes. At vortex closure, the fluid
will still be circulating in the blender and will
appear to fold away from the blender sides To test the crosslinking delay and the
into the center of the cup. There may still be a crosslinking delay temperature, you will need
depression in the fluid surface at the center of the following items:
the cup, but the vortex that remains is very little.
• Waring blender
STEP 05 Continue mixing the fluid. Record • 4 plastic cups
the time at which the fluid surface stops moving
and forms a small dome at the center of the • glass beaker
blender cup. This time is the crowning time. • pH meter
• thermometer
5.4 Fracturing fluid crosslink delay
• timer
Crosslinking is a chemical reaction allowing a
continuous, 3D structure to form in a fluid under • fluid sample.
the right conditions. Crosslinking reactions There are numerous ways to determine the
are delayed to reduce friction pressure during crosslink delay time and crosslink delay
pumping and to reduce the time a crosslinked temperature of hydraulic fracturing fluids.
fluid is exposed to high shear rates. Most Unfortunately, the most commonly employed
metal-crosslinked polymer fluids are irreversibly methods are highly subjective. This JET manual
destroyed when they are exposed to high shear outlines the basic procedures used for these
rates after crosslinking. subjective tests.
The delay between adding the crosslinkers and

the actual crosslinking is the crosslink delay Note:
time. Any factor that affects the dissolution rate Be careful to follow these
(such as temperature, concentration, shear procedures exactly. Subtle
rate, particle size distribution) will change differences in the initial conditions
the crosslink delay. Typically, fluids that use and the mixing steps will change
dissolving particles are time delayed. the results.
It is also possible to add additives that interfere

with the interaction between the crosslinker
and the polymer until the fluid temperature
increases. The temperature at which
crosslinking will occur is called the crosslinking
delay temperature.

Sample preparation record the temperature. Take 15 sec or less for
this mixing and temperature measurement step.
You will repeat the following steps to prepare
samples for the crosslink delay time and the
crosslink delay temperature tests. STEP 03 Repeat Steps 01 and 02 as
necessary. Record the temperature at which
the following three characteristics are evident.
STEP 01 Prepare 250 mL of the fracturing
fluid following the procedure set forth in the 1. Initially, the fluid begins to thicken. It
relevant section of the Fracturing Materials may remain linear or it may become
Manual. stringy and cling to the thermometer.
However, it manifests this stage,
the fluid is now substantially more
Note: viscous than the linear gel was.
Do not add the last ingredient Some call temperature at which this
(typically the crosslinker and/ point is reached the initial crosslink
or buffer) until the initial fluid temperature.
temperature and pH are measured.
2. The fluid can support a pencil-thick
tongue hanging off the edge of the
beaker. The point at which it is possible
STEP 02 Measure the initial fluid
to pull the tongue back into the beaker
temperature and pH, and record these values.
is the crosslink temperature. This is
the temperature that should be used
STEP 03 Add the last ingredient, probably for designing the crosslink delay
the crosslinker and/or buffer, to the fracturing temperature for treatments.
fluid and mix in the Waring blender at
2,000 rpm for 30 sec. The crosslink delay 3. The fluid becomes dry (usually) and
time measurement starts as soon as the last can support a broad, thick tongue
ingredients are added to the fluid; record this hanging off the edge of the beaker. The
time. Measure the final fluid pH during this step. temperature at which this occurs is the
full dry crosslink temperature.
Crosslink delay temperature
Follow these steps to determine the crosslink
delay temperature. 5.5 Static gel break test
The static gel break test determines the time
STEP 01 Transfer the entire contents of at which the gel breaks enough to flow back.
the blender cup into a glass beaker. Place the A gel is usually considered broken enough to
beaker into a microwave oven and heat the fluid flow back when it has degraded to a viscosity
for 10 sec. of 20 cp at the required temperature. This test
is important for the field operation that does not
have high-pressure, high-temperature (HPHT),
STEP 02 Remove the cup and briefly stir gel break test equipment.
the fluid with a thermometer at a rate similar
to whipping eggs with a whisk. Then, allow the To perform the static gel break test for any
thermometer to equilibrate with the fluid and temperature, you will need the following items:

• 1,000 mL jar with cap
STEP 08 Tighten the cap.
• 200 mL high temperature bottles
• HPHT fluid loss cell and heating jacket STEP 09 Shake the jar vigorously every
30 min and visually observe the viscosity.
• Fann 35 rheometer with proper accessories
• water bath with temperature control STEP 10 Install the Fann 35’s rotor, bob,
• thermometer and sample cup. Heat the sample cup.
• stop watch STEP 11 Take enough of the gel from the
• gel and breaker sample. jar to fill the sample cup and place it into the
heated sample cup.
Follow these test procedures for
temperatures less than 100 degC. STEP 12 Place the thermometer into the
sample.
STEP 01 Prepare the base gel. STEP 13 Watch the thermometer closely.
Start testing the fluid viscosity at 170 sec-1 as
STEP 02 Place the required amount of quickly as possible when the fluid temperature
breaker solution into the linear gel before is at the required temperature (the BHT). The
adding the crosslinker solution. Dissolve J218 Fann 35 does not have heating capabilities,
or J481 into a small amount of water; use so the sample should be heated to BHT in the
equivalent amounts of J218 and J481 if J475 water bath.
and J490 Encap-breaker are used and refer
to the Fracturing Materials Manual, InTouch
STEP 14 Continue the process in step 03
until fluid viscosity reaches 20 cp. Write the
Content ID# 4223817, for the Encap breaker
time required to reach this viscosity, which is
release rate. the static gel break time.
STEP 03 Crosslink the gel according to fluid Follow these test procedures for
preparation procedures that are published for temperatures greater than 100 degC, using
that particular gel. a HPHT fluid loss cell.
STEP 04 Preheat the water bath to the

STEP 01 Prepare the base gel.
required temperature. STEP 02 Place the required amount of
breaker solution into the linear gel before
STEP 05 Pour 500 mL of gel into the jar. adding the crosslinker solution. Dissolve J218
Replace the cap. or J481 into a small amount of water; use
equivalent amount of J218 and J481 if J475
STEP 06 Place the jar containing the gel
and J490 Encap-breaker are used, and refer to
FMM for Encap-breaker release rate.
in the water bath that will bring the sample to
the required temperature. Stir it slowly while STEP 03 Crosslink the gel according to the
heating, to accelerate the crosslinking process. fluid preparation procedures.
STEP 07 Start the timer when temperature STEP 04 Preheat the heating jacket to the
reaches the indicated bottomhole temperature required bottomhole static temperature (BHST).
(BHT).

STEP 05 Place the crosslinked gel into the To perform this test, you will need the following
bottle and finger-tighten the cap. Put the bottle items:
with the sample into the HPHT cell containing
the proper level of oil just below the bottle cap • Fann Model 50-type viscometer with
connection, to avoid oil getting into the bottle appropriate parameters (speed factor, R-B
and contaminating the fluid. Keep the whole cell factor, and spring factor)
assembly vertical while putting the bottle into
• rotor and bob-5 or bob-5X. Different bobs
the HPHT cell.
will have different shear rate ramps. For
example, shear rate ramp corresponds
STEP 06 Place the HPHT cell assembly to 118 rpm, 88 rpm, 59 rpm, 88 rpm, and
with bottle/oil heating medium into the heating 118 rpm with a B5 bob.
jacket; again, keep all components vertical.
• fracturing fluid sample.
STEP 07 Start the timer when the HPHT Follow these test procedures. They could vary
cell temperature reaches the indicated BHT. with different types of machine.
STEP 08 Visually observe the viscosity of STEP 01 Power on the viscometer and its
the fluid by cooling down the cell and taking out computer.
the bottle at the expected breaking time. Using
your laboratory experience, determine whether STEP 02 Supply water and N2 (usually at
it has broken or not. If it doesn’t break, you will 450 psi, or 800 psi for Encap-breaker) after the
have to repeat the test with more breaker. machine is calibrated properly.
5.6 HPHT gel rheology STEP 03 Prepare the crosslinked fracturing

fluid as described in the specific fracturing fluid
A Fann Model 50-type viscometer is used for
laboratory preparation procedures.
performing a crosslinked gel breaking test
when a BHT above 100 degC is required (see
Fig. 5- 2). STEP 04 Activate the viscometer computer
program and select Operating Menu, then Heat
Bath. Type in the required temperature to start
preheating the oil bath.
STEP 05 Place about 26 mL (for a bob- 5)

of the crosslinked gel inside the rotor cup,
followed by the required amount of breaker.
STEP 06 Place approximately 26 mL more

of the crosslinked gel into the rotor cup.
STEP 07 Screw the bob counterclockwise

to the shaft until it is finger tight.
Figure 5-2. Fann Model 50 Viscometer

STEP 08 Slowly screw the rotor containing STEP 17 Allow the machine to cool down
the sample to the expansion fitting until it is below 100 degF. Release the pressure and
finger tight. close the water line.
STEP 09 Take off the cover of the oil bath STEP 18 Dissemble the rotor cup and
and close the glass door. bob gently and clean them up using the
recommended cleaner.
STEP 10 Go to the Operating Menu, and
then Custom (or API). The API ramp should be STEP 19 Turn on the nitrogen to 10 to
one of the following: 20 psi to get all excess water or gel residue out
of the expansion fitting.
• 118 rpm (100 sec-1)
• 88.5 rpm (75 sec-1) STEP 20 Spray some WD40 on the shaft
• 59 rpm (50 sec-1) to lubricate the bearing. Use a paper towel to
wipe the moisture and gel off the shaft very
• 29.5 rpm (25 sec-1) gently (do not press against the shaft). Clean
• 59 rpm (50 sec-1) everything used and cover the oil bath.
• 88.5 rpm (75 sec-1)

STEP 21 Turn off the machine and release
• 118 rpm (100 sec-1). the pressure in the main nitrogen line.
STEP 11 Choose bob5, interval stir rate

(118 rpm), and final temperature setpoint. 5.7 Fracturing sand sieve analysis
The sand used as a proppant must be analyzed
STEP 12 Click Initial test in the operating for size of the grains. You will use a series of
menu followed by Yes and OK to go to ASCII sieves that are stacked in a specified order; see
FILE and report printout. Choose the options Fig. 5-3.
you need.
STEP 13 Follow the screens through until

Perform Test appears; click it.
STEP 14 The instrument will automatically

run until the program finishes and prints out the
results.
STEP 15 If you want to stop the machine

during testing, go to the operating menu and
select Shut down.
STEP 16 Click on the file on the top of Figure 5-3. ASTM Standard Sieves and
Endecotts Sieve Shaker
screen and find the reprint report. Click it to
print out the report manually.

5.7.1 Sampling techniques 5.7.2 Sand sieve analysis (modified API
A proper sampling ensures that a method)
representative sample of the fracturing sand is This method has been modified to meet specific
obtained for quality control testing. criteria requested by clients. This method
exceeds the API recommended practice 56 for
• delivery samples sand sieve analysis.
○ Nine samples are needed per railroad
car; 3 samples per truck load; 5 samples STEP 01 Refer to API RP56 or Table 5-4 to
per 100,000 lbm when on location. determine the recommended sieve sizes used
○ When the proper number of samples are in testing designated sand sizes.
obtained, combine the samples for one
test. Table 5-4. Recommended Sieve Sizes for Fracturing Sands
Fracturing sand size designations
• conveyor belt samples
USA sieves recommended
○ Sand falling from a conveyor belt into a 6/12 8/16 12/20 16/30 20/40 30/50 40/70 70/140
truck or railcar should be allowed to flow
4 6 8 12 16 20 30 50
for at least 2 minutes before catching
sample; wait 2 minutes after the start 6 8 12 16 20 30 40 70
of each compartment when catching 8 12 16 20 30 40 50 100

location samples.
10 14 18 25 35 45 60 120
○ Place the sampling device in the 12 16 20 30 40 50 70 140
stream of sand with its longitudinal axis
16 20 30 40 50 70 100 200
perpendicular to the flowing sand. Move
the sampling box at a uniform rate from pan pan pan pan pan pan pan pan
side to side in the sand stream. Several

samples should be extracted at uniform
intervals through the body of sand and
combined for a representative sample.
STEP 02 Establish an accurate weight (wt)
of the 100-g split sample to within 0.1 g.
• alternate sampling method (non-API): If a
flowing sample is not possible or desired, STEP 03 Make sure that all sieves are
then a grain thief may be used to obtain completely cleaned with the manufacturer-
a sample. It is recommended to catch at recommended brush. Weigh each sieve
least three samples whenever possible and accurately and record the weights.
combine them for testing.
STEP 04 Stack the sieves in order of
increasing mesh size from bottom to top, with
the pan on the bottom.
STEP 05 Pour the sample onto the top

sieve and place the sieve set plus the pan in
the test sieve shaker. Cover the sieves and
tighten the sieve set.

STEP 06 Power on the sieve shaker for 5.8 Proppant turbidity test
10 min. The turbidity test is performed to determine
the cleanliness of the fracture sand (amount of
STEP 07 Remove each sieve and weigh fines present).
each sieve separately with its contents. Weigh
the pan also. You will need the following equipment and
materials:
Note: • sand sample

Remember to brush off the
• distilled water
particles from the bottom of each
sieve into the next size sieve before • glass medicine bottle graduated to 100 mL
weighing either. with cap
• black felt tip permanent marker
• small funnel to pour sand into medicine
bottle.
Follow this procedure to test the turbidity:
STEP 08 Calculate the percent by weight
of the total sand sample retained on each sieve
and the pan. To calculate the percentage by STEP 01 Mark the flat side of the bottle with
weight of the sand falling within the designated an X using the black felt tip marker.
sieve sizes, use these equations:
• weight of the retained sand (WR) = sieve

STEP 02 Fill the bottle to the 20-mL mark
with sand.
weight after shaking – sieve weight before
shaking
STEP 03 Add distilled water to the 100-mL
• wt% of the total sand sample retained on mark and secure cap.
each sieve = WR/WT x 100.
STEP 09 A minimum of 90 wt% of the STEP 04 Shake the bottle vigorously for
tested sample should fall within the designated 20 sec.
sieve sizes. Not more than 1.0 wt% of the total
tested sand sample should be larger than the STEP 05 In a well-lit area, hold the bottle
largest sieve size and not more than 1 wt% at arms’ length with the flat side away from
should be smaller than the smallest sieve size. yourself.
If the X can be seen clearly, the sand

Note: passes the turbidity test. If the X is barely
The cumulative weight should be distinguishable or cannot be seen, the sand
within 0.5% of the sample weight fails the test.
used in the test; if not, the sieve
analysis must be repeated using a
different sample.

Note: STEP 04 Dial the program number #750
and set the wavelength to 450 nm.
After the turbidity test is complete,
check the pH of the sample; if the
pH is above 6.0, the sand will be STEP 05 Zero the FTU using DI water in
acceptable for YF1XX and YF2XX the test vial.
series fluids.
STEP 06 Using a syringe or pippet, extract
25 mL of water-silt suspension from near the
center of the water volume.
5.9 Silt turbidity test
Turbidity in water is the result of suspended STEP 07 Place the water-silt suspension in
clay, silt, or finely divided inorganic matter being the test vial.
present. The HACH DR 2000 spectrometer
measures the optical property of the
suspension, providing a turbidity value for the
STEP 08 Determine the sample turbidity in
FTU and record.
tested proppant sample. The turbidity of the
tested proppant sample should be 250 (FTU)
formazine turbidity units or less. 5.10 Proppant sphericity and roundness
Particle sphericity is a measurement of how
closely a sand particle or grain approaches the
shape of a sphere. Grain roundness is a mea-
• HACH DR 2000-type spectrometer
sure of the relative sharpness of grain corners,
• sample vials or of grain curvature. Figure 5-4 illustrates
• 6-oz or larger, plastic-capped, widemouth these concepts.
bottle
The test method is specified by API RP56 /60
• syringe/pippet (Krumbein and Sloss visual estimation method).
• DI water
• proppant sample.
Follow these procedures.
STEP 01
Sphericity
Measure 20 mL of dry proppant

sample and 100 mL of DI water in a 6-oz
widemouth bottle, mix well, and allow to stand
for 30 min.
STEP 02 Shake the bottle vigorously by

hand for 45 to 60 shakes in 30 sec. Allow it to
Roundness
stand for 5 min.
Figure 5-4. Sphericity vs. Roundness
STEP 03 Switch on the spectrometer.

To test for sphericity and roundness, you will To test the fluid’s compatibility with the RCP,
need the following equipment. follow these procedures.
• optical microscope Heerbrugg, Model
Wild M3 or scanning electron microscopy
STEP 01 Prepare 500 mL of linear gel plus
(SEM), Phillips, Model XL30 all additives except crosslinker. The crosslinker
is not added for zirconate crosslinked fluids to
• sample sticker/platform
prevent shear degradation during compatibility
• proppant sample. test.
To perform the test, follow this procedure.
STEP 02 Measure pH using pH meter.
STEP 01 Stick 20 or more grains of
proppant on the glass plate platform for STEP 03 Add 10 ppa of RCP, and mix for
electronic scanning electron microscope 30 sec at a mixer speed that creates a vortex
(ESEM). without significantly entraining air.
STEP 02 Switch on the optical microscope. STEP 04 Place the mixture in a water bath
Refer to the SEM analysis for ESEM startup at 150 degF for 30 min.
procedures.
STEP 03 Adjust the magnification until a STEP 05 After 30 min, remove the mixture
clear picture of proppant particles shows up. from the bath and mix for 30 sec more. Stop
blender and allow proppant to settle to bottom
STEP 04 Compare the shape of the of container.
particles visually with the standard chart (see
API RP56, p. 7) and determine the sphericity STEP 06 Transfer 250 mL of fluid (without
and roundness of each particle. proppant) Note:
to a clean blender.
STEP 05 Record the average of the above Allow fluid to cool before
reading as the sphericity and roundness of the continuing.
proppant sample.
5.11 Fluid compatibility with RCP STEP 07 Measure pH using pH meter.
Laboratory testing is performed to determine STEP 08 Add crosslinker and perform the
the compatibility of RCP with fracturing fluids. bench top and rheology tests described here,
or use the Fracturing Materials Manual. Follow
relevant quality control standard procedures.
• pH meter
STEP 09 Compare fluid properties
• water bath and rheology profile with that of a fluid not
• Waring blender exposed to RCP. Viscosities measured on
• linear gel sample a Fann 50-type rheometer should be similar
for fluids prepared with and without RCP
• all additives exposure (typically within 100 cp for same test
• RCP sample conditions).
• fluid not exposed to RCP.

then quickly screw the upper and lower halves
STEP 10 If significant loss in viscosity is
together.
observed, fluid performance may be improved
by increasing the crosslinker concentration.
STEP 03 Immerse the apparatus into the
If significant loss in viscosity is observed—the water bath and start heating. Heat bath slowly
fluid is not stable and looks broken—you will so that the sample temperature remains close
know that the fluid is not compatible with the to the bath temperature.
RCP.
STEP 04 Using the Reid vapor pressure
tester, record vapor pressure of the sample
5.12 Vapor pressure test when the temperature is 100 degF. Note the
The Reid method determines the vapor exact temperature and pressure when taking a
pressure of petroleum products. This method reading.
offers the type of data commonly requested for
the field. Be sure to shake the test chamber vigorously
before each reading to ensure that the validity
of the sample has been maximized.
Warning:
Keep heat and ignition sources STEP 05 Continue heating and record the
away from the test. vapor pressure when the bath temperature
reaches 130 degF. Note the exact temperature
and pressure at the time of the reading.
STEP 06 Discard the sample and
• sample to be tested thoroughly wash the apparatus with water.
Note: STEP 07 To find the vapor pressure, plot

Sample should be handled pressure vs. temperature of the data collected.
diligently to minimize vapor loss. Extrapolate to obtain the exact pressure at
100 degF and 130 degF for reporting.
• water bath, adjustable from 100 to

140 degF
• Reid vapor pressure tester; refer to
ASTM232-82 for details.
Follow this procedure.
STEP 01 Unscrew the testing chamber at

its midsection and inspect the O-ring seal.
STEP 02 Transfer 25 to 30 mL of sample

to the bottom half of the testing chamber and

6.0 Hydraulic Fracturing Fluids
These hydraulic fluids are the fluids that the

engineer designs for a particular job. They must
STEP 04 Add the required amount of
polymer to the blender, mixing at 2,000 rpm.
be tested in the laboratory before pumping the
job. These procedures explain preparing the
fluids. STEP 05 Mix for 5 min.
STEP 06 Measure viscosity at 100 rpm on

6.1 Linear gel a Fann 35 with R1-B1 at 80 degF.
The linear gel (Fig. 6-1) can be prepared for all
water-base fluids in this way.
Figure 6-1. Sample Linear Gel
To prepare the linear gel, follow these generic

procedures.
STEP 01 Measure 500 mL of deionized (or

field) water into a 1-L Waring blender cup.
STEP 02 Add either 167 ppt KCl or

2 galUS/1,000 galUS L64. You may need to
stir until well mixed, depending on the specific
fracture fluid.
STEP 03 Adjust the fluid pH if necessary,

as per the manual guidelines for your specific
fluid.

6.2 YF1xxHTD fluids • L10 crosslinker 7.5 lbm/1,000 galUS
(0.45 g)
The Widefrac* 100HTD (YF*100HTD) fracturing
fluids are water-base systems comprising • M2 activator 15 lbm/1,000 galUS (0.9 g)
a refined guar gelling agent crosslinked • J450 stabilizer 1 galUS/1,000 galUS
by a borate-type crosslinker. These fluids (0.5 mL)
are designed for batch- or continuous-mix
operations. • J480 crosslink delay agent in concentration
to be determined
YF100HTD fluids can be used at temperatures • J490 encap-breaker, in concentration to be
ranging from 125 to 325 degF (52 to 163 degC). determined.
To prepare YF1xxHTD, you will need the Prepare the YF1xxHTD according to the
following items: following procedure.
• Waring blender equipped with variable Prepare linear gel:

transformer
STEP 01 Pour 490 mL of water into the
• blender jar mixing cup. Stir with low speed.
• graduated cylinder and syringes
• timer STEP 02 Add 10 g of KCl and 0.027 g of
M275 into the mixing cup.
• magnetic stirrer
• glass bottle, 1L STEP 03 Add 2.4 g of J424 slowly into
the cup and control the stir rate to allow the
• pH meter
polymer to disperse.
• thermometer
• Fann 35-type viscometer. STEP 04 Increase the stir rate after the
polymer disperses to hydrate faster.
You will also need the proper additives. The
additives in a typical YF140HTD system can
include the following (concentration amount for STEP 05 Hydrate the gel for 30 to 60 min.
500 mL):
STEP 06 While the gel is hydrating, weigh
• M117 potasium chloride 166 lbm/ 0.6 g of J353 and dissolve it in a small amount
1,000 galUS (10 g) of water.
• M275 microbiocide 0.45 lbm/1,000 galUS
(0.027 g) STEP 07 Check the fluid temperature and
pH of the gel. The pH should be 6 to 8.
• J353 HT gel stabilizer 10 lbm/1,000 galUS
(0.6 g)
STEP 08 Check the fluid viscosity to
• F103 surfactant 1 galUS/1,000 galUS see if it is in the range specified in the FMM
(0.5 mL) specification. See Fann 35 test procedures in
• J424 gelling agent 40 lbm/1,000 galUS, Section 5.2, Linear fluid viscosity.
(2.4 g)
38 | Hydraulic Fracturing Fluids

Prepare the crosslinker: STEP 17 Add the prepared crosslinker into
the linear gel while start timing.
STEP 09 Put 3.7 mL of water into a glass
bottle. Stir using magnetic stirrer.
STEP 18 Record the time to reach the
vortex closure as the vortex closure time.
STEP 10 Weigh 0.9 g of M2 and add slowly
into the bottle while stirring.
STEP 19 Check the time until hang-lip
happens and record this time as the hang-lip
STEP 11 Measure 0.45 g of L10 and add it time.
into the bottle while stirring.
STEP 12 Add the required amount of J480

STEP 20 Check the pH of the crosslinked
gel and record.
slowly while stirring, until dissolved.
STEP 13 Place 0.5 mL of J450 into the

bottle.
STEP 14 Age the crosslinker solution for

60 min.
Crosslink the gel (see Fig. 6-2):
Figure 6-2. Crosslinked Gel
STEP 15 Adjust the stirring speed to create

a vortex to the tip of the stirrer.
STEP 16 Add J353 solution and 0.5 mL of

F103 into the mixing cup to mix 1 min.

6.3 YF8xxHT fluids Follow this procedure to prepare the YF845HT.
YF800HT fluids are temperature-activated, Prepare linear gel:
zirconate-crosslinked, water-base fluids
that use carboxymethylhydroxypropyl guar
(CMHPG) as a gelling agent. Crosslinker J515
STEP 01 Pour 490 mL of water into the
mixing cup. Stir with the Waring blender on low
is used to crosslink the fluids. There are two
speed.
fluid designs:
• YF800LPH (pH 4 to 5) for temperatures STEP 02 Leaving the blender on, add 10 g
from 100 degF to 250 degF [38 degC to of KCl and 0.027 g of M275 into the mixing cup.
121 degC]
• YF800HT (pH 9 to 9.5) for temperatures STEP 03 Measure 5.05 mL of polymer
from 275 degF to 350 degF [135 degC to slurry (J916) and add slowly into the cup.
177 degC]. Control the stir rate to allow the polymer to
disperse.
To prepare YF800HT, you will need the
following equipment and materials:
STEP 04 Add L401 while checking the pH
• Waring blender equipped with variable of the fluid until the pH is 7.0. Record the pH.
transformer
• jar STEP 05 Increase the stir rate to obtain
faster hydration and hydrate for 30 min.
• pH meter STEP 06 Check the fluid viscosity to see
• thermometer if it is in the specified range. Record the linear
viscosity against FMM spec, the pH (6.9 to 7.1),
• Fann 35-type spectrophotometer. and the temperature.
The following additives are often used in a
typical YF845HT (concentration amount for STEP 07 While the gel is hydrating, weigh
500 mL). Check that these or any others 0.6 g of J353 and 0.6 g of J464. Dissolve each
indicated are in stock. using approximately 2 mL of water, in separate
containers.
• M117 potasium chloride 166 lbm/Mgal: 10 g
• M275 microbiocide 0.45 lbm/Mgal: 0.027 g
• F103 surfactant 1 galUS/Mgal: 0.5 mL Note:
The J464 solution will be used later
• J916 gelling agent 10.1 galUS/Mgal: in this procedure.
5.05 mL
• L401 buffer: adjust to pH 6.5–7.0
• J353 HT gel stabilizer 10 lbm/Mgal: 0.6 g STEP 08 After the gel hydrates to meet the
specification, add the J353 solution and then
• J464 activator 10 lbm/Mgal: 0.6 g 0.5 mL of F103 surfactant into the linear gel, in
• M2 (2%) activator 10 galUS/Mgal: 5 mL that order. Stir the gel for approximately 2 min,
and then check the pH again.
• J450 stabilizer 1 galUS/Mgal: 0.5 mL
• J515 crosslinker 0.7 galUS/Mgal: 0.35 mL

Crosslink the gel: STEP 15 Shake the fluid frequently to
avoid a temperature gradient from the wall of
STEP 09 Heat the water bath to the beaker to the center of the fluid. Check the
approximately 90 degC or use a microwave crosslink every 15 to 30 sec (adjust the time
oven for homogeneous heating. more frequently while using the microwave;
especially when close to the desired
temperature) while testing the fluid temperature
Note: by thermometer. Record the fluid temperature
Using the microwave is the when there is a noticeable resistance to the
recommended practice. thermometer moving into/out of the fluid.
6.4 YF”GO”-III fluid

STEP 10 Add J464 solution, M2 (2%),
0.5 mL of J450, and 0.35 mL of J515 into the YF“GO”III* is a gelled, oil-base fluid used as
linear gel. Check the pH after adding each a fracturing fluid for the treatment of water-
component. sensitive formations. Diesel, kerosene,
condensate, and a wide variety of crude oils
can be used to prepare YF“GO”III.
STEP 11 Continue to mix the fluid at a
vortex to the tip of the stirrer for 30 sec after
To prepare the YF“GO’’III, you will need the
adding the J515. Check the fluid pH.
STEP 12 Split the prepared mixture into two • disposable syringes

equal parts of approximately 250 mL. You will
use one part to perform the crosslinking test • glass or plastic beakers
and the other part to perform the Fann 50 test. • magnetic stirrer
• balance
STEP 13 Begin the Fann 50 test as soon as
possible after mixing the fluid in Step 11. The • Waring blender
time between the end of the fluid mixing and • Fann 35 viscometer
beginning the Fann 50 test should not be more
than 5 min. • graduated measuring cylinders
• water bath
STEP 14 To perform the crosslinking test, • J452 oil gelling agent
place the beaker containing 250 mL of prepared
gel into the water bath or microwave. • J601 crosslinker
• J602L pH control agent
• M003 breaker.

Follow this procedure. Table 6-1. J452 and Activator for YF”GO”III Gel
J452 (mL/1,000 mL Activator (mL/1,000 mL
diesel) diesel)
Note:
6 3
If J602 is to be used, mix 1.44 g of
J602 solid in 10 mL of deionized 7 3.5
water until it dissolves. This solution
is equivalent to J602L. 8 4
STEP 04 Mix at 10,000 rpm for 10 min.

STEP 01 Mix J602L and J601 at a ratio of
1:5 by volume. STEP 05 Transfer gel to a Fann 35 cup and
measure viscosity developed at 170 sec-1. Table
Place a small glass beaker on the magnetic
6-2 shows the desired viscosities for 6, 7, or
stirrer and add the following additives:
8- galUS gels.
• J602L: 2 mL Table 6-2. Desired Viscosities
• J601: 10 mL Viscosity (cP @ 170 sec-1
J452 (mL/1,000 mL)
@ 21 degC)
Allow this solution to mix for at least 30 min.
6 100 to 120
STEP 02 Place 1 L of the base fluid, usually 7 120 to 140

diesel, in a Waring Blender and start mixing at
8 140 to 170
2,000 rpm. Create a vortex down to the blades.
Note: 6.5 YF100LG fluids

Normally the base fluid is diesel The Widefrac* 100 (YF100LG) fracturing
containing <0.5% water because fluids are water-base systems comprising a
the system is water sensitive. refined guar gelling agent crosslinked by a
borate crosslinker. They are prepared from
the Waterfrac 100 fluids. YF100LG fluids
STEP 03 Simultaneously add the desired are designed to crosslink quickly. The vortex
quantity of J452 and the activator solution closure of these fluids is 5 to 10 sec, which
prepared in Steps 01 and 02 to the edge of the allows uniform mixing of all components before
vortex. The quantities required to produce 6, becoming viscous. The crosslink is fairly mature
7, or 8 galUS of gel per 1,000 galUS of diesel in another 10 to 20 sec.
(6, 7, or 8 mL/1,000 mL) are listed in Table 6-1.
To prepare the YF100LG solution, you will need
the following equipment and materials:
• Waring blender
• blender cup
• graduated cylinders

• disposable syringes Continue mixing for 15 to 20 min until the solids
have dissolved.
• pH meter or paper
• water gelling agent J424 or PSG polymer
slurry J877. Note:
The specific gravity of a 16%
Prepare YF100LG solution.
(wt/wt) solution at 75 degF is
1.131 g/cm3. An addition rate of
STEP 01 Add crosslinker L010 at 1.2 to 11.3 mL/1,000 mL of linear gel
2.2 lbm L010/1,000 galUS WF100 fluid (0.144 to is equivalent to 12 lbm J494 and
0.264 g L010/L) depending on the temperature. 5 lbm M3/1,000 galUS of fluid.
For adding small quantities, a stock solution of
L010 can be prepared by mixing 2.3965 g of
L010 to 100 mL of distilled water.
Prepare breaker solution:
STEP 05 A stock solution of J218 can be
Note: prepared by adding 2.3965 g of J218 to 100 mL
1 mL L010 stock solution per of distilled water. Then, 1 mL J218 stock
200 mL of WF100 = 1 lbm solution per 200 mL of WF100 = 1 lbm J218/
L010/1,000 galUS WF100. 1,000 galUS WF100.
STEP 06 Prepare 500 mL of WF100 base

gel.
Activate crosslinker: STEP 07 Add L010 to the base gel and mix
at low speed for 1 min, checking to ensure that
STEP 02 The pH stabilizer (activator air is not trapped in the gel.
solution) for fracturing temperatures less
than 175 degF (79 degC) contains J494 at STEP 08 If J218 breaker is required, add
12 lbm/1,000 galUS of YF fluid and M3 at the required amount to the vortex and mix for
5 lbm/1,000 galUS of YF fluid. This is called a 1 min.
12-5 solution.
STEP 09 Set the mixer speed to 1900 to
The preferred way to add the J494 and M3 2000 rpm and add 5.65 mL of the J494:M3
to the fluid is to prepare a 14 to 20% (wt/wt) activator solution to the vortex. A vortex closure
aqueous solution and meter it in the blender. of 10 to 15 sec should be observed.
To prepare a 16% (wt/wt) 12-5 solution, first
place 19 mL of deionized water in a small glass STEP 10 After 30 sec, stop the mixer and
beaker on a magnetic stirrer. transfer the fluid to a beaker. The fluid should
be fully crosslinked.
STEP 03 Slowly add 2.55 g of J494 to the STEP 11 Check the pH of the crosslinked
vortex. fluid. It should be 9.6 to 9.9 at ambient
temperature. If it is not, you may have
STEP 04 Slowly add 1.06 g of M3 to the contaminated additives and will need to repeat
vortex. the test with fresh additives.

6.6 YF100LGD fluid • L10: 7 lbm (0.84g)
Widefrac 100LGD (YF100LGD) fracturing fluids • M2: 16.5 lbm (1.98g)
are water-base systems containing a refined • J450: 1 galUS (1 mL)
guar gelling agent (20 to 50 lbm/ 1,000 gal)
crosslinked with a borate crosslinker. This example solution, before the J450 is
YF100LGD fluids can be batch-mixed or added, has a specific gravity of 1.304 at
continuous-mixed. YF100LGD fluids are 24 degC and therefore will have an addition rate
prepared from any of the Waterfrac 100 of 7.8 galUS/1,000 galUS (or 7.8 mL/1,000 mL),
(WF100) fluids. Addition of crosslinker, calculated as follows:
activators and a delay agent converts the
WF100 fluid to the corresponding YF100LGD • Crosslinker rate
fluid. = (weight of crosslinker solution/
1,000 galUS)/(8.34 x SG)
To prepare the YF100LGD solution, you will = [(6 x 8.34) + 7 + 16.5]/(1.304 x 8.34)
need the following equipment and materials: = 6.8 galUS/1,000 galUS with 1
galUS/ 1,000 J450
• Waring blender = 7.8 galUS/1,000 galUS (1.56 mL/200 mL)
• blender cup Mix crosslinker delay solution:
• graduated cylinders STEP 02 The concentration of the

• disposable syringes delay agent J511 depends on the polymer
concentration, mix water temperature, and the
• pH meter or paper desired crosslink time
• water gelling agent J424 or PSG polymer
slurry J877. The minimum J511 concentration required
to prevent syneresis (over-crosslinking) at
Follow these procedures to mix the solution.
room temperature for approximately 12 hr is
10 lbm/1,000 galUS. J511 is readily soluble
Prepare crosslinker:
in water. The addition of NaOH at about 1
lbm/1,000 galUS prevents bacteria from
STEP 01 Mix the crosslinker solution
deteriorating the J511 solution (resulting in
according to the specific requirements. The
~pH 10). Aqueous solutions with 30 to 70%
crosslinker solution comprises the following:
J511 present can be employed. To prepare a
• water (4.5 to 7 galUS/1,000 galUS). 30% solution containing 2.79 lbm J511/galUS,
add 0.02 g of J511 to 70 mL of water and mix
• L010 at 5.5 to 9.0 lbm L010/1,000 galUS until it is dissolved.
WF100 fluid (0.659 to 1.078 g L010/L)
depending on temperature.
• activator M2 (10 to 20 lbm/1,000 galUS) or
U28.
• stabilizer J450, typically 1 galUS/
1,000 galUS (if required).
For example,
• fresh water: 6 galUS (6 mL)

STEP 03 Add 30 g of J511 and continue STEP 04 Inject the crosslinker solution and
mixing until all solids have dissolved. Table 6-3 start the stopwatch simultaneously.
can be used as a guideline for adding various
quantities of J511. STEP 05 Vortex closure is defined by
the crosslinked gel covering the blade nut.
Table 6-3. Quantities of J511 in YF100 LGD Record the time elapsed between injecting the
Equivalent crosslinker solution and vortex closure.
Desired Equivalent
to galUS of
concentration
30% J511/
to mL of 30% STEP 06 Stop the blender and pour the gel
J511 (lbm/ J511/200 mL into a 250-mL beaker. Start the stopwatch.
1,000 galUS of
1,000 gal US) of WF100
WF100
STEP 07 Pour the fluid from one 250-mL
10 3.6 0.72 cup to another until 80% crosslink is achieved.
15 5.4 1.08 The 80% crosslink is defined by the floppy gel
easily retracting into the cup and showing no
20 7.2 1.44 adhesion to the wall of the cup when the gel is
25 8.9 1.78
poured.
30 10.7 2.14 Also, notice if the crosslinked gel can be

fractured during the floppy test. Record the
Prepare breaker solution: time elapsed from vortex closure to 80%
crosslinking.
STEP 04 Prepare a breaker solution by
STEP 08 Continue pouring the crosslinked
adding 2.3965 g of J218 or J481 to 100 mL of
distilled water. gel from cup to cup every 15 sec until 100%
crosslinking is achieved. The 100% crosslink
1 mL J218 or J481 stock solution per 200 mL is defined as when the crosslink gel is poured
of WF100= 1 lbm J218 or J481/1,000 galUS from cup to cup, the fluid comes out in one solid
WF100 mass with minimal elongation.
6.7 Crosslink delay 6.8 PrimeFRAC fluids

To determine the crosslink delay time with The PrimeFRAC* fluids are temperature-
various concentrations of J511 present, the activated, zirconium-crosslinked waterbase
following procedure should be followed: fluids composed of CMHPG. PrimeFRAC fluids
are designed to be crosslinked with J513 in a
pH range from 9.1 to 9.5 in the temperature
STEP 01 Place 200 mL of the prepared range of 200 degF to 350 degF.
WF100 fluid into a Waring blender jar and
record the fluid temperature. You will need the following equipment and
materials:
STEP O2 Start mixing at 2,000 rpm; this
speed should produce a vortex. • Waring blender equipped with variable
transformer
STEP 03 Inject the delay agent and mix for • blender jar
2 min.

• pH meter STEP 06 Check the fluid viscosity to
• thermometer determine if it is in the specified range
according to the Fann 35 test procedures.
• Fann 35
Record the linear viscosity against the Fracture
• microwave Materials Manual specifications (170 sec-1 and
511 sec-1), pH, and temperature.
• titrator
• 0.1N HCl STEP 07 Continue mixing for another 5 min
• methyl orange indicator until the viscosity meets the specification.
• phenolphthalein indicator
• water 6.8.1 Crosslinking and delay times
• Orion Model 130A conductivity meter To determine the PrimeFrac gel crosslinking
and delay times, follow this procedure.
• fluid additives and RCP.
Follow these procedures to prepare the system. STEP 01 Fill blender with 250 mL of the
prepared linear gel; shear at low speed.
STEP 01 Check the pH of the water. It
should be 6 to 8; adjust by HCl or NaOH if not STEP 02 Add J464 solution, J494 solution,
in this range. and J513 into the linear gel. Check pH after
adding each component.
STEP 02 Pour a small amount of water into
the mixing cup. Stir with low speed. Add D047 if STEP 03 Continue to mix the fluid at a
required. vortex (to the tip of stirrer) for 20 to 30 sec after
adding J513.
STEP 03 Add required KCl, M275, F103,
and J353 in this sequence into the mixing cup. STEP 04 Check and record the fluid pH.
STEP 04 Measure polymer slurry and add STEP 05 Split the prepared mixture into two
slowly into the mixing cup. Control the stir rate equal parts. You will use one part to perform
to allow the polymer to disperse. Check the pH the crosslinking test and the other part to
of the fluid while adding J488 until the fluid pH perform the Fann 50 test.
is less than 7.0; record the pH and the amount
of J488 needed to reach this pH. STEP 06 Start the Fann 50 test as soon
as possible after mixing the fluid. The time
STEP 05 Increase the stir rate to hydrate between the end of mixing the fluid and
the gel faster, and hydrate for about 10 to beginning the Fann 50 test should not be more
15 min. than 5 min.
STEP 07 To perform the crosslinking test,

place a beaker containing 150 mL of prepared
gel into the microwave.

STEP 08 Check the crosslinking every 5 J464L and repeat the procedure if the crosslink
temperature does not meet the specification of
to 10 sec while testing the fluid temperature by
thermometer. less than 120 degF. Otherwise, go to next step.
STEP 09 Write down the fluid temperature STEP 09 Put approximately 35 mL of the
when there is a noticeable resistance to the fluid into a beaker and add the required breaker
thermometer moving into/out of the fluid (100% to perform the Fann 50 tests.
crosslinked). This temperature should be less
than 120 degF for better fluid stability. STEP 10 Increase the amount of proppant
added for the FracCADE design to check all
loadings (for example, 2 ppa, 4 ppa, 6 ppa,
6.8.2 RCP/PrimeFRAC compatibility 8 ppa, 10 ppa, and 12 ppa). Repeat Steps 01
To determine the compatibility between the through 09 to obtain a detailed relationship
PrimeFRAC solution and the RCP, follow this between the RCP loading and the gel
procedure. crosslinking/gel stability.
STEP 01 Fill the blender cup with 250 mL of 6.8.3 QA/QC for J464L, J494L, and J513
the prepared linear PrimeFRAC gel.
Follow these procedures to check the quality of
the J464L, J494L, and J513 PrimeFrac fluids.
STEP 02 Add required amount of J464L For all these fluids, you will need the following
and J494L, mix at low speed. equipment and materials:
STEP 03 Add 1 ppa RCP to the blender; • beakers

increase mixing speed for deep vortex to shear • conductivity meter
for 2 to 3 min.
• pH meter
STEP 04 Add J513 into the blender in the • methyl orange indicator
last few seconds during shearing. • phenolphthalein indicator
• 0.1N HCl
STEP 05 Let mixture settle for about 2 min.
• DI water
STEP 06 Mix at 1,500 rpm for 3 to 5 min. • fluid sample.
STEP 07 Decant the clear part of the

mixture. Check pH to make sure it is in the
range of 9.2 to 9.5. If it is not, adjust with J494L
to meet the pH requirement and record the
amount of J494L added and the final pH.
STEP 08 Put approximately 150 mL

of the gel into the beaker and place it into
the microwave to determine the crosslink
temperature according to the procedure in
Section 6.8.1. Change the concentration of

6.8.3.1 J464L • mL of 0.1N HCl x 0.1786 = lbm of
J494/ galUS
To verify the quality of J464 at 0.50 lbm/galUS,
follow this procedure. The fluid is acceptable if the concentration is
within ±10% of specification.
STEP 01 Dilute 1 mL of J464L sample in The engineer may adjust the field J494L rate
50 mL of DI water. based on the results of this test.
STEP 02 Add 4 drops of methyl orange

indicator and shake until the mixture is 6.8.3.3 J513
homogeneous. To verify the quality of J513 solutions, follow
this procedure.
STEP 03 Titrate with 0.1N HCl standard
solution until the color changes from orange
to pink. The endpoint should be approximately
STEP 01 Prepare standard J513 solutions
of 15%, 25%, 35%, and 50%, using 100 mL of
6.7 mL.
location water to dilute the J513.
STEP 04 Calculate the concentration:

STEP 02 Measure the conductivity of the
• mL of 0.1N HCl x 0.0742 = lbm of J464/ standard J513 solutions using the conductivity
galUS meter.
STEP 05 The fluid is acceptable if the within STEP 03 Prepare a standard curve of
±10% of specification. conductivity vs. temperature for various J513
concentrations.
STEP 06 Adjust field J464L rate based on
above results. STEP 04 Measure the conductivity of the
field-prepared J513 solution.
6.8.3.2 J494L
STEP 05 Determine the volume % of J513
To verify the quality of J494 at 1 lbm/galUS, for the field-prepared J513 solution from the
follow this procedure. standard curve (additional check on SG should
be completed to verify the field sample)
STEP 01 Dilute 1 mL of J494L sample to
approximately 50 mL of DI water. STEP 06 Calculate the concentration of
J513 in the field sample. It is acceptable if
STEP 02 Add 4 drops of phenolphthalein within ±10% of specification.
indicator and shake until homogeneous (turns
pink).
Note:
The volume % J513 determined in
STEP 03 Titrate with 0.1N HCl standard
Step 06 = galUS J513/galUS of the
solution until fluid color changes from pink to
field sample.
colorless (endpoint, about 5.6 mL).
STEP 04 Calculate the concentration:

6.9 Super X emulsion You will need the following equipment and
materials:
Super X Emulsion (SXE*) is a viscous,
highly retarded, concentrated acid system • 350-mL glass beakers
designed for use in matrix acidizing or acid
fracturing of carbonate formations. SXE is • syringe
an oil-external phase emulsion formed with a • 15-mL glass tubes
70:30 hydrochloric acid-to-oil ratio, stabilized
with an emulsifier. Hydrochloric acid (HCl) • magnetic stirrer
concentrations ranging from 15% to 28% • PMC hot-plate stirrer with speed
may be used. SXE is designed for batch-mix adjustment
operations; however, continuous-mix operations
can be performed by following the procedures • Fann 35 with Hestolloy bob/sleeve and fluid
provided in the field mixing procedures cup
section. The temperature range of SXE is 75 • kerosene or diesel
to 375 degF [23 to 191 degC] and emulsion
• HCl, 7.5% to 28%
breakout times can be customized by varying
the emulsifying agent U108 loading as needed. • A166 corrosion inhibitor
U108 replaces both U080 (low temperature • U080 emulsifying agent
emulsifier for SXE) and U103 (high temperature
emulsifier for SXE-HT). • glass rod
• 2% KCl.
Follow this procedure to mix the SXE.
Caution:
Goggles, rubber gloves, and a
protective covering must be worn STEP 01 Add 140 mL HCl into glass beaker
when mixing acids. Always work and mix with the magnetic stirrer at a speed
under a fume hood when preparing high enough to produce a vortex with the
acids. stirrer bar. Add the A166 corrosion inhibitor as
required and mix until homogeneous.
STEP 02 Place another beaker on the

Warning: mixing plate and place 60 mL each of kerosene
Always add concentrated acid to and U080 into the beaker to mix thoroughly with
water. Do not add water to the acid a vortex tip to the bottom of the beaker.
because the resulting heat could
make the acid boil up onto your STEP 03 Use a syringe to drop the acid and
skin or eyes. inhibitor mixture into the oil and U080 mixture
while stirring with the tip of the vortex to the
beaker bottom.
STEP 04 Increase the mixing speed as

high as the mixer can mix, after adding all acid
mixture into the oil mixture, for about 15 to
20 min.

STEP 05 A stable emulsion system should • thermometer
be prepared. Place a small sample of the • Fann 35
emulsion into a 15-mL glass tube to observe
• additives commonly used in ClearFRAC
for 10 min. No separation will be evident if the
systems (example concentration amount in
emulsion is an oil-external stable emulsion.
500 mL):
Another way to check the oil-external property ○ M117 potassium chloride 333 lbm/Mgal
is to tick a drop of emulsion using the glass rod 20 g
and drop it into a 2% KCl solution in a 15-mL
glass tube. If an oil-external emulsion forms, the ○ J508W gelling agent 4.0 galUS/Mgal
drop will remain and slowly settle down to the 2.0 mL
tube bottom; otherwise, the drop will disperse ○ J463 (T>150F) HT activator 5 lbm/Mgal
quickly into the solution. 0.3 g.
Follow this procedure to prepare the solution.
Some commercial diesel is contaminated and
not suitable for SXE preparation. If you are
having difficulty forming a stable oil-external STEP 01 Pour 500 mL of water into the
emulsion, change the source of the oil. blender jar and stir.
STEP 06 When you obtain a stable oil- STEP 02 Test the fluid temperature.
external emulsion, check the rheology using
the Fann 35 with the Hestolloy bob/sleeve STEP 03 If the fluid temperature is less than
combinations. 150 degF, add 20 g of KCl and dissolve it. If the
fluid temperature is greater than 150 degF, add
0.3 g of J463 and dissolve it.
6.10 ClearFRAC J508W
ClearFRAC* fracturing fluids are water-base
systems comprising a viscoelastic surfactant
STEP 04 Create a vortex to the tip of
the stirrer. Slowly add J508 into the mixture.
(J508W) and a brine. Full fluid viscosity is The amount of J508 used will depend on the
achieved once the surfactant is completely desired viscosity.
dispersed in the brine. Viscosity develops
rapidly without shear degradation. ClearFRAC
fluids can be batch mixed or continuous mixed. STEP 05 Stir the mixture until the vortex
Maximum fluid temperature is 240 degF. closes.
To prepare a ClearFRAC solution, you will need STEP 06 Place the mixture into the water
the following equipment and materials. bath at 70 to 80 degC to get the foam out. The
fluid should become clear.
• Waring blender equipped with variable
transformer STEP 07 Check the fluid temperature and
• blender jar pH.
STEP 08 Check the fluid viscosity to see if
• timer it is in the specified range.
• pH meter

7.0 Matrix Acidizing Fluids
Matrix acidizing fluids are used in acidizing 7.1 HCl

treatments. Table 7-1 shows the acidizing
systems most used by Schlumberger. The maximum concentration of commercial HCl
is 36%. Table 7-2 lists the hydrochloric acids
Table 7-1. Acid Systems Most Used by Schlumberger most used in the oilfield industry. Use this table
to prepare 1000 mL of different dilutions of HCl
Major application Acid systems from 36% HCl.
Carbonate acidizing Hydrichloric acid
Intensified acid Table 7-2. Dilutions of Concentrated Hydrochloric Aicd
Mud acid 36% HCI
Clay acid HCI Acid
Sandstone acidizing needed Density g/cc)
Organic mud acid Strength
Organic clay acid (mL)
Alcoholic acid 28% 751 1.141
Gas well Gas well acid
Gas well mug acid 20% 507 1.099
Retarded acid DAD acid
SXE/SXE HT 15% 379 1.074
Gelled acid LCA/SDA/VDA 10% 247 1.049

BDA 7.5% 183 1.036
Mud removal MSR
NARS 5.0% 120 1.024
Organic damage removal Clean sweep
Scale dissolving CAS U104/U105/U106 To prepare 1,000 mL of any concentration of

HCl, follow this procedure.
Aqueous acetic acid
Perforating acid Formic acid
Perforating acid STEP 01 Place approximately 200 mL of
water in a 1,000-mL volumetric flask.
The following sections describe how to prepare
laboratory samples of these acid systems. STEP 02 Add the required quantity of
concentrated HCl (see Table 7-2) into the flask
very slowly.
Caution:
Heat and odor will be released. It
is strongly recommended that this
procedure be performed in a fume
hood.

Caution: • HCl base acid
Always remember to add acid to
• required inhibitor
water. Never add water to acid.
• Y001 (33.8 lbm/1,000 galUS).
STEP 03 Finish filling the flask to the
graduated line indicating 1,000 mL. STEP 01 Place the required amount of HCl
base acid with the required amount of inhibitor
STEP 04 Cap the flask and shake it a few into a plastic beaker.
times upside down over a sink or in the fume
hood. STEP 02 Stir the solution until
homogeneous with the magnetic stirrer.
7.2 Intensified Acid
Intensified acid is a regular inhibited HCl STEP 03 Add the required amount of Y001
(generally 15%) with 33.8 lbm/1,000 galUS (33.8 lbm/1,000 galUS) slowly.
Y001 (0.25%) added.
STEP 04 Stir the mixture until the solution
becomes clear.
Note:
Y001 is ammonium bifluoride, 7.3 Clay acid
which combines with water to form
HF acid. Clay acids from Schlumberger are designed
specifically for acidizing sensitive sandstone
formations. They not only provide good
stimulation, but also provide permanent
It is often used in initial cleanup as well as stabilization of clays and other fines, eliminating
in dolomitic limestones containing a certain water sensitivity and the mobility of migratory
amount of silica. As much as 50% more fines. Clay acids slowly release hydrofluoric
reaction occurs between intensified acid and acid (HF) from the hydrolysis of fluoboric acid
dolomitic limestone at surface conditions. (HBF4) and can penetrate a much greater
The increase is less pronounced at elevated distance from the wellbore before spending
temperatures. Field results also confirm the than mud acid can. There are four formulations
value of intensified acid as a cleanup treatment of clay acid presented here:
in dolomitic limestone formations.
• full strength clay acid
A side reaction product of CaF2 precipitate • full strength clay acid LT (low-temperature
could cause damage. formulation)
To mixing intensified acid, you will need the • half-strength clay acid
following equipment and materials: • half-strength clay acid LT.
• plastic beaker large enough to hold the Clay acids are the only acid formulations that
acid, inhibitor, and Y001 require shut-in time. One reason is that they
slowly release HF, limiting the amount of HF
52 | Matrix Acidizing Fluids

available at any one time. Another reason for Table 7-3. Formulations for Clay Acids
shut-in time is the unique feature of borosilicate, Full strength
a reaction product, to coalesce and form a Half-strength
clay acid
coating on undissolved particles. This coating Ingredients clay acid, H913
H813
of borosilicate will cement the affected clays (SG 1.047)
(SG 1.096)
and fines in place, thus severely limiting further
Water 680 mL 843 mL
clay migration in the contact area.
Y100 120 g 60 g
Clay acids are generally used from 130 degF to
300 degF, but clay acids LT are only used from 35% HCI 194 mL 97 mL
100 degF to 130 degF. Y006 60 g 30 g
To mix clay acids, you will need the following:
• glass beaker Table 7-4. Formulations for Low-Temperature Clay Acids

Full strength
• magnetic stirrer Half-strength
Ingredients clay acid LT
clay acid, H914
• water H814
• Y001 Water 545 mL 772 mL
• L010 Y100 120 g 60 g

• HCl. 35% HCI 336 mL 168 mL
To mix a clay acid, refer to Tables 7-1 and 7-2 Y006 60 g 30 g
for additives and quantities. Each formulation
prepares 1,000 mL of clay acid. S.G. 1.121 1.047
Note:
7.4 Mud acid
To prepare clay acid properly, the
additives must be added in the Mud acid is a mixture of inhibited HCl acid
order listed in the table (from top to and hydrofluoric acid. Mud acid can not
bottom); otherwise, a precipitate will only dissolve the minerals that HCl acid can
form. dissolve, but it can also dissolve siliceous
minerals presented in most sandstone
formations.
Note:
Y006 and L010 have the same Note:
composition and can directly Calcium, magnesium, sodium, and
replace each other. potassium brines can react with HF
acid to form insoluble precipitates.
Do not use any of these for mixing
the solution.

To mix mud acids, you will need the following
equipment and materials:
Caution:
• plastic beaker Wear safety goggles, protective
clothing, and rubber gloves. Work
• magnetic stirrer in a fume hood.
• water
• Y001
• HCl. STEP 01 Place the appropriate quantity of
Table 7-5 lists the additives and quantities fresh water in a plastic beaker.
required to prepare the most common mud acid
formulations.
Note:
Do not use seawater, oilfield brine,
Caution: calcium, magnesium, potassium, or
Because of the safety issues sodium chlorides to prepare mud
associated with concentrated HF acid.
acid, it is strongly recommended to
mix the mud acid with the quantities
of Y001 inhibitor listed in the table. STEP 02 Add the required amount of Y001.
Mix using a magnetic stirrer until the Y001 has
dissolved completely.
To mix mud acid according to Table 7-5, follow

this procedure. STEP 03 Add the required quantity of
concentrated HCl slowly. Mix until clear.
Table 7-5. Mud Acid Formulations

Concentration 36% HCI (mL) Y001 (g) Water (mL) Density (g/cc)
4% HCI – 0.5% HF 110 7.2 885 1.022

6% HCI – 0.5% HF 160 7.2 835 1.032
8% HCI – 0.5% HF 210 7.2 785 1.041
6% HCI – 1% HF 170 15 820 1.036
8% HCI – 1% HF 220 15 770 1.045
10% HCI – 1% HF 270 15 720 1.054
6% HCI – 1.5% HF 180 24 804 1.041
7.5% HCI – 1.5% HF 220 24 764 1.048
10% HCI – 1.5% HF 290 24 694 1.061
12% HCI – 1.5% HF 340 24 644 1.07
10% HCI – 2% HF 300 30 680 1.065
12% HCI – 3% HF 380 48 588 1.085

The formula for preparing 1,000 mL is as
follows:
Caution:
Heat will be generated! Be sure • fresh water
always to add acid to the water–
never add water to the acid. • inhibitor as required
• 48 g Y001
• 72 mL 36% HCl
7.5 Organic mud acid • A186
Organic mud acid is a mixture of 9% formic • 90 mL L36.
acid (HCO2H; also called L36) and 3% HF acid.
It is more easily inhibited, has a lower reaction Follow this procedure to mix organic mud acid.
rate, and has less tendency to form asphaltic
sludge than HCl acids. STEP 01 Add approximately of fresh water
in the plastic beaker. Set magnetic stirrer to a
Organic mud acid is recommended for use in speed high enough to form a vortex.
high-temperature matrix acidizing and wellbore
damage removal in both sandstone and
carbonate reservoirs where extended inhibition
STEP 02 Add A186 and mix thoroughly.
time is expected and asphaltic sludges are
formed when the formation contacts HCl acids. STEP 03 Add the Y001 into the beaker
slowly and stir until totally dissolved.
Warning: STEP 04 Add the HCl acid and L36. Stir

Both Y001 and L36 can cause until the mixture is homogenous.
severe eye and skin burns. Wear
the proper PPE. STEP 05 Fill up the container to the
1,000- mL line with fresh water.
To mix organic mud acids, you will need the

• 1,000-mL plastic beaker

• water
• A186
• Y001
• HCl.

7.6 Organic clay acid • lowers the surface tension
An organic clay acid (OCA) system is used for • increases the vapor pressure and improves
acidizing sandstones containing high silt/clay postclean up effectiveness
content and for HCl-sensitive formations. It • retards the acid reaction rate and improves
reduces secondary precipitation and fines success in acidizing low to medium
migration after the treatment. It can remove permeability dry gas formations
formation damage caused by clay and other
aluminosilicate minerals, and it can be used for • slightly accelerates the corrosion rate.
high temperature applications. The concentration of alcoholic acid mixtures
indicates the volume percentage of each
Tables 7-6 and 7-7 list two OCA formulations additive in the acid. For example, an 80:20
(OCA-R and OCA-HT) and the conditions alcoholic acid mixture is prepared by mixing
under which they should be applied. 800 mL of acid (e.g., 15% HCl) and 200 mL of
alcohol.
Table 7-6. OCA Formulations
Component OCA-R OCA-HT
Note:
HCI 5% 1.5% When the mixture mentioned in the
J285 5% 5% text is prepared, there is a volume
loss of 10 mL.
L001 13.4% 10%
Y001 5% 2%
Y006 2.5% 1.2%
Table 7-7. Conditions for Using OCA Formulations

Conditions OCA-R OCA-HT
>300F - *
<300F, silt/ * -
clay>30%
>5% zeolite - *
<5% zeolite * -
>5% chlorite - *
<5% chlorite * -
* Fluid applicable under this condition
- Fluid not applicable under these conditions
7.7 Alcoholic acid

Alcoholic acid is a mixture of acid (HCl or
mud acid) and alcohol (F003 or K046). Adding
alcohol into the acid

7.8 Dynamic acid dispersion (DAD) STEP 03 Continue mixing while slowly
A dynamic acid dispersion (DAD) is an adding acid through the hole in the blender
acid outside-phase emulsion stabilized cup lid. Add a volume equal to the volume of
with dispersing agent U074. The dispersion the P121 and the U074 mixture prepared in
simultaneously dissolves the minerals and Step 02.
removes the oily paraffinic deposits.
STEP 04 Increase the speed of the Waring
The dispersion can be prepared with various blender to around 1,000 rpm. Mix for 10 min.
acids and hydrocarbon solvents. HCl and P121 An oil-outside phase dispersion should form.
(toluene) are the most common. Ratios of acid: The fluid will have some viscosity and may stick
hydrocarbon can be made from 10 to 50%. to the sides of the blender cup. This is the seed
Usually 15 galUS of U074 per 1,000 galUS of batch dispersion.
acid is used to stabilize the emulsion.
To mix a DAD, you will need the following

STEP 05 Continue mixing slowly, and
steadily add the acid solution through the
equipment and materials: hole in the blender lid to the seed batch. The
emulsion should invert to become acid-outside
• Waring blender phase. The fluid should wet the sides of the
• 1,000-mL glass beaker blender cup and easily drain down the sides of
the cup.
• HCl acid
• appropriate corrosion inhibitor STEP 06 Mix 15 min more at 1,000 rpm.
• P121.
Use this procedure to mix a DAD.
Note:
The DAD cannot be stored for long
Caution: durations.
The fumes are hazardous. Prepare
the DAD under a fume hood or use
appropriate precautions. Wear all
appropriate PPE.
STEP 01 Prepare 450 mL of 15% HCl acid.

Add appropriate corrosion inhibitor for suitable
protection time.
STEP 02 Place 50 mL of P121 in a Waring

blender cup. Add the required quantity of U074.
Set the speed on the blender to create a vortex
down to the blades of the blender. Mix for
3 min.


8.0 QA/QC Practices
All fluids used in fracturing treatments must be you should have one proppant sample for
tested to ensure quality and conformance with every 50,000 lbm of proppant.
the design requirements. The following sections
• Check field additives for pH, appearance,
describe QA/QC procedures for these tests.
and odor. pH paper may be used for
additives, but if a problem is observed,
8.1 Fracture fluid QA/QC double check the additive with the pH
meter.
The following tests are required:
• Prepare a base gel for each fracture tank
• Perform API water analysis on all location and check (i.e., if there are six tanks, then
water samples. Analysis will include pH and six linear gel tests must be performed).
chloride, carbonate, bicarbonate, and iron The base gel viscosity must fall within the
concentrations. acceptable range before ANY rheological
characteristics are measured. Fluid pH will
• Perform silicate analysis for all also be checked with a pH probe to ensure
PrimeFRAC, YF800HT, and YF800LpH the proper pH range (6.0 to 8.0) for polymer
fluids. Silicates should be less than hydration.
25 ppm.
• Verify crosslinked gel properties (pH
• Perform bacteria analysis upon measured using a pH probe, initial crosslink
request. Bacteria should be less than temperature, and gel lip test) for each
3,000,000 per L. fracture tank before measuring rheological
• Test all concentrated KCl tanks for total properties. The initial crosslink temperature
hardness. Total hardness should be less should be within 2 degF of the requested
than 400 ppm. value.
• Test all unfamiliar water sources (e.g., pond • Evaluate the crosslinked gel viscosity using
or lake water) and low polymer systems composite water samples and a Fann 50-
(e.g., PrimeFRAC) for total hardness. Total type rheometer at 100 sec-1.
hardness should be less than 400 ppm.
• Total hardness strips can be used to Note:
analyze the hardness of water. If the total If there are fewer water samples
hardness strips indicate values of 425 or than requested Fann tests, then do
greater, use the Hach kit for more accurate not use composite samples.
determination. The strips are not reliable for
high concentrations.
• Perform sand sieve analysis on all • Composite samples are to be prepared
proppant samples. Of the proppant, 90% using no more than three water samples for
must fall within the screen size specified for a single composite sample (i.e., composite
that proppant for a particular job. Typically, 1 can be made up of samples from tanks 1,
2, and 3; while composite 2 can be made

up of samples from tanks 4, 5, and 6, but ○ Changes in the fluid design or problems
no composite can be made up of samples with the testing must be communicated
from 4 or more water samples). Use to the laboratory manager and the
different composite samples for different fracturing department.
Fann runs to be sure that all water samples
○ If the laboratory cannot correct poor
are tested. Use 52-mL samples and
test results, the fracturing department
API RP39 procedures unless otherwise
must be notified directly. The laboratory
specified.
report should include results, description
of problem, and likely source/solution of
Note: problem.
45-mL samples can be used when High rheology data (e.g., in excess of 1,500 cp
bob-climb problems are observed. for nonramp or nonspike data) may indicate
Perform tests for 20 min longer overdesign of fracturing fluid and the fracturing
than the job pump time. department should be notified.
The fracturing fluid design test results will be

• Perform break tests with live active plotted on a standard format. The report will be
breakers using a Fann 50-type rheometer. sent to the field or sales engineer requesting
When using encapsulated breakers, the tests.
800- psi overburden pressure is preferred
to minimize nonrepresentative release of
breaker (400 psi is the minimum pressure 8.2 Fracture fluid additives QA/QC
regardless of breaker type). To minimize
Field additives must be checked for pH,
testing, crosslinked gel can be tested with
appearance, and odor. pH paper may be used
the appropriate amount of encapsulated
for additives, but if a problem is observed,
breaker and be considered similar to those
double check with the pH meter. The pH
in the absence of breaker, provided the
should fall within the range listed in Table 8- 1
coating is stable at test temperature.
for common fracturing additives. If additive
• The current rule of thumb for determining problems are suspected, then measure
the lifetime of a fracturing fluid is the time conductivity and specific gravity. Measure
at which the viscosity falls below 100 cp at conductivity for all crosslinkers and titrate all
a shear rate of 100 sec-1 (300 cp at a shear buffers and activators to determine actual
rate of 40 sec-1, or 80 cp at a shear rate of concentration.
170 sec-1), or below a requested level.
• Location water should be used for
determining break times. Source water can
be used if location water is not available
with sufficient time for laboratory testing. In
such case, a test should be performed with
location water to verify test results.
• Problems with laboratory testing should
be communicated with senior laboratory
personnel and the fracturing department.
60 | QA/QC Practices
Table 8-1. Physical Properties of Various Fracturing Fluid Additives
Additive Description pH Range Color Specific gravity Conductivity
[mS at 70 degF]
F103 Surfactant 5 to 7 Colorless 0.94 53 to 63
F103/W54 50:50 mixture 5 to 7 Clear–yellow 0.94 0.7 to 1.7
F104 Foaming agent 7 to 9 Clear–amber 1.02
F802 Surfactant 6 to 7 Amber 0.92

blend
J353L High 7 to 9 Light yellow 1.3 128 to 135
temperature gel
stabilizer
J450 Stabilizer 11.5 Colorless 1.12
J464L Buffer 8 to 9.5 Colorless 1.03 34 to 36

(0.5 lbm/galUS)
J488 Acid buffer 5.5 to 6 Colorless 1.09 to 1.13 62 to 65
J494L Buffer (1.0 9 to 11 Colorless 1.06 to 1.08

lbm/galUS)
J508W Viscoelastic 6 to 9 Yellow–brown 0.93
sufractant
J511 Delay agent 6 to 7 Clear 1.07 to 1.12
solution
J513(25%) Zirconate 6 to 7 Yellow–brown 1.05 38 to 40
crosslinker
J515(25%) Zirconate 6 to 7 Yellow–brown 1.05 15 to 17
crosslinker
J877 HPG diesel 6 to 7 (paper) Amber 1.06 to 1.09 –
slurry
J916 CMHPG diesel 6 to 7 (paper) Amber 1.06 to 1.09 –
slurry
L010 Solution 3 wt% borate 4 to 6 Colorless 1.02 0.3 to 0.6
crosslinker
L064 KCI substitute 5 to 7 Colorless 1.01 62 to 85
L401 Acid buffer <4 Colorless 1.02

(acetic acid)
LGD X/L Borate >13 Colorless 1.22 220
Solution crosslinker (0.7
ppg L10, 0.5 gpg
U28)
U028 (10%) Caustic >10 Colorless 1.04
W054 Nonemulsifying 6 to 7 Clear–yellow 0.88

g agent

8.2.1 J515 Table 8-2. Specific Gravity of J515 Dilutions and Conductivities
To prepare the J515 test solution, you will need J515 Dilution Conductivity
Specific gravity
the following equipment and materials. [volume %] at 70 degF
5 5.7 1.01
• 100-mL volumetric flask 12.5 10.2 1.03
• Orion Model 130A conductivity meter 20 13.7 1.04
25 15.6 1.05
• local water
35 18.2 1.07
• J515 sample. 50 19.6 1.08
Follow this procedure. 100 (raw) ~14 1.22
STEP 01 Prepare standard J515 solutions STEP 05 Calculate the concentration of

(e.g., 15, 25, and 35%) using the 100-mL J515 in the field sample. The J515 fluid is
volumetric flask and the local water to dilute the acceptable if its concentration is within ±10% of
J515. specification. To find the concentration to use in
the field sample, use this equation:
STEP 02 Measure the conductivity of
the solutions using the Orion Model 130A • (volume % J515 determined in Step 5)/100
conductivity meter. Prepare a standard curve = galUS J515/galUS of the field sample
of conductivity reading versus temperature for
various volume% J515. 8.2.2 LGD Crosslinker
To test LGD crosslinker, you will need the
STEP 03 Measure the conductivity of the following equipment and materials:
field-prepared J515 solution.
• beaker
STEP 04 Determine the volume % J515 for • Orion Model 130A conductivity meter
the field-prepared solution from the standard
curve. An additional check of the specific • local water
gravity should be completed to verify the field • LGD crosslinker.
sample. Table 8-2 shows the SG for specific
dilutions and conductivities. Follow this procedure.
STEP 01 Prepare a standard LGD

crosslinker solution of 0.7 ppg L010, 0.5 gpg
U028, and 0.45 gpg water, using the local
water.
STEP 02 Measure the conductivity of

the test solution using an Orion Model 130A
conductivity meter. Prepare a standard curve of
conductivity reading versus temperature.
STEP 03 Measure the conductivity on the

field-prepared LGD crosslinker solution.
STEP 04 Compare the conductivity of the
field-prepared LGD crosslinker solution with the
standard curve.
For this test solution, if the conductivity at

70 degF is 220 mS, the specific gravity should
be 1.22. Complete an additional check of the
specific gravity to verify the field sample.
8.2.3 U028
To test the quality of a U028 fluid, you will need
the following equipment and materials:
• beaker
• DI or distilled water
• U028 sample
• 0.1N HCl acid
• phenolphthalein indicator.
STEP 01 Dilute 1 mL of U028 sample to

approximately 50 mL using distilled or deionized
water.
STEP 02 Add 3 drops (0.25 mL) of

phenolphthalein indicator (pink to colorless
endpoint).
STEP 03 Titrate with 0.100 N HCl to the

clear/colorless endpoint.
STEP 04 Calculate concentration of U028:
• 0.100 N HCl (mL) = % U028

The fluid is acceptable if the concentration of
U028 is within ±10% of specification. The field
engineer can adjust the field U028 add rate
based on the concentration.

9.0 References
These sources will provide more information on

stimulation laboratory procedures:
• Well Services Safety Standard 24:

Laboratory Operation, InTouch Content
ID# 3313702
• Key Service Quality Requirements for
Stimulation, InTouch Content ID# 4147783
• Fracturing Engineering Manual Section
900, Acid Fracturing, InTouch Content ID#
3015576
1200 Appendix B –Fracturing Fluids,
InTouch Content ID# 3015580
1300 Appendix C –Additives, InTouch
Content ID# 3012434
• Fracturing Materials Manual volume I and
II: Fluids InTouch Content ID# 4223817
• Matrix Materials Manual, InTouch Content
ID# 4013354
• Stimulation client support lab procedures
and information, InTouch Content ID#
3948499.

66 | References
10.0 Check Your Understanding
1. Choose all true statements regarding eye 2. Select two correct statements regarding
protection in the laboratory. protective clothing in the laboratory
A. Safety glasses with fixed side shields A. Laboratory coats with long sleeves
are required at all times as minimum must be worn.
eye protection (does not apply to B. Rubber or plastic protective aprons
offices, rest rooms, or other protected must be worn, depending on the type
areas not in the laboratory working of chemical. Read the MSDSs for the
area). protective clothing requirements.
B. Indirect vented chemical goggles must C. Types of clothing that allows exposure
be worn when handling chemicals such to a large area of skin can be worn in a
as cement, unless these chemicals are laboratory, e.g., sleeveless tops, short
in sealed containers. skirts, or short pants.
C. Face shields must be worn when D. Safety boots are not required in
handling hot liquids, acids, or liquids the laboratory. Shoes that provide
that are under pressure, working with protection from liquids must be worn,
flammable liquids where the flash point such as a leather shoe that covers the
is less than 100 degF. foot. Sandals and open shoes are not
D. Visitors must wear safety glasses with permitted.
side shields while in the laboratory work
areas.
3. Which of the following quality assurance
E. All of the above are true. tasks should be done on location before
pumping?
A. Check the amount of water in each
tank, take water sample from each
tank, and test the samples.
B. Test linear gel viscosity from the outlet
of the PCM/GelSTREAK.
C. Check all the amounts of additives;
recalculate to make sure enough for
the job is available.
D. Test the crosslinker and all additives.
E. All of the above are true.

4. Which of the following quality assurance 7. Which statements are true regarding
tasks should be performed during specific gravity?
pumping? A. Specific gravity is the ratio of the
A. Throughout the job, the linear gel weight of material to the weight of
should be continually checked for water, or the density of the material to
viscosity and temperature to confirm the density of water.
the proper gel loading of the gel. B. The higher the specific gravity is, the
B. Samples should be taken from the heavier the liquid is.
outlet of the blender or fracture pumps C. Specific gravity can be used
to test the delay time of the cross- to differentiate hydrocarbons
linked fluid as well as pH, temperature, (condensate) from water. Fresh water
bottomhole temperature stability, and has a specific gravity of 1.000.
break testing (water bath).
D. A hydrometer is the device used to
C. The physical quantities of all liquid and measure specific gravity.
dry additives should be continually
checked throughout the job to compare E. All of the above are true.
to the designed amount to be pumped.
D. All of the above should be done. 8. Alkalinity tests include _________ .
A. SG and pH tests
5. Choose the correct statement regarding B. bicarbonates, carbonates, and
API gravity. hydroxide test
A. The equation relating specific gravity to C. all of the above
API gravity is D. none of the above
SG= 141.5
131.5 + API
9. Choose all correct statements about
B. The higher the API gravity is, the bicarbonates.
heavier the fluid is. A. Bicarbonates are very important for
C. The higher the API gravity is, the lighter fracture fluid quality control.
the fluid is. B. Fracturing fluids require various
D. Both A and C are true. bicarbonate concentrations, depending
E. None of the above is true. on the specific fluid.
C. High bicarbonates will tend to slow gel
hydration and delay fluid crosslinking.
6. Which statement regarding pH is
incorrect? D. High bicarbonate levels may be
characterized by a high pH or be an
A. The normal pH range for brines is
indication of carbonates present in the
between 6 to 8.
water.
B. The normal pH range for fracture fluids
is 11 to 12.
C. A low pH may indicate spent acid.
D. A high pH may indicate contamination
by mud or filtrate.
68 | Check Your Understanding

10. Choose the correct statement(s) regarding 14. Choose all true statements regarding iron:
carbonates and hydroxides: A. When high iron is encountered in
A. Most formations contain high levels of fracture mix water, breaker J218
carbonates or hydroxides. (ammonium persulfate) will have an
B. If the water sample contains carbonate accelerated effect.
and/or hydroxide, it may be a clue B. In high iron environments, J218
to a problem in the customer’s well, may cause premature break of the
possibly indicating the presence of fracturing fluid.
some drilling mud contamination. C. High iron content will interfere with
C. Most oilfield waters will contain the crosslinking of the fracturing fluid,
only bicarbonates, but occasionally resulting in poor crosslink integrity.
carbonate and/or hydroxide will be D. The maximum iron concentration for
present. fracture water ranges from 8 ppm to
D. None of the above are true. 25 ppm, depending on the fluid.
11. Choose the correct statement about
chloride. 15. Which instrument is used to determine
A. Most fracture fluids today comprise 2% viscosity of linear fluids?
KCl. A. spectrophotometer
B. The chloride content of a 2% KCl B. Fann® Model 35 rheometer (Fann35)
solution should be approximately
9,600 mg/L. C. hydrometer
C. The chloride test can also be used to D. none of the above

determine if a sample is spent acid.
D. All of the above are true. 16. What is the vortex closure test?
A. The vortex closure test indicates the
12. How would you identify H2S in the onset of viscosity development, and
sample? rarely coincides with full crosslinking.
A. The water sample is very cloudy. B. The vortex closure test indicates full
crosslinking.
B. The sample smells like rotten eggs.
C. None of the above are true.
C. The sample has large particles floating
in it.
D. None of the above are true.
13. The hardness tests include a test for

_________.
A. sulfur and magnesium
B. calcium and magnesium
C. calcium and potassium
D. sodium and potassium

17. What are three distinct fluid behaviors D. none of the above
during a vortex closure test in the order in
which they occur?
20. What is the proppant turbidity test used
1. fluid crowning, which is the formation for?
of a dome of fluid over the center of the
A. to determine the shape of the sand
blender cup (over the blades). This is
the point at which the fluid no longer B. to determine the cleanliness of the
completely circulates in the blender fracture sand (amount of fines)
cup C. to determine the toughness of the sand
2. viscosity increase that results in D. none of the above
closure of the vortex, but does not stop
fluid circulation in the blender cup
21. Which statement is true about the
3. linear fluid behavior, characterized by a
fracturing fluids?
deep vortex
A. The Widefrac 100HTD (YF*100HTD)
fracturing fluids are water-base systems
___ A. 1, 2, 3 comprising a refined guar gelling
___ B. 2, 3, 1 agent crosslinked by a borate-type
crosslinker.
___ C. 3, 2, 1
B. YF800HT fluids are temperature-
___ D. 1, 3, 2
activated, zirconate-crosslinked water-
base fluids that use CMHPG as a
18. Which statement is true regarding the gelling agent.
static gel break test? C. YFGOIII is a gelled, oil-base fluid used
A. The static gel break test tests for the as a fracturing fluid for the treatment
time at which the gel breaks enough to of water-sensitive formations. Diesel,
flow back. kerosene, condensate, and a wide
B. A gel is usually considered broken variety of crude oils can be used to
enough to flow back when it has prepare YFGOIII.
degraded to a viscosity of 20 cp at the D. All of the above are true.
required temperature.
C. This test is important for the field 22. Which is true about SXE (Super X
operation that does not have high- Emulsion)?
pressure, high-temperature (HPHT) gel
A. SXE is a viscous, highly retarded,
break test equipment.
concentrated acid system designed for
D. All of the above are true. use in matrix acidizing or acid fracturing
of carbonate formations.
19. What instrument is used to perform a B. SXE is an oil-external phase emulsion
crosslinked gel breaking test when a BHT formed with a 70:30 HCl-to-oil ratio,
is above 100 degC? stabilized with an emulsifier.
A. a Fann Model 35 type rheometer C. HCl concentrations ranging from 15%
B. a Fann Model 50 type rheometer to 28% may be used.
C. a Waring blender D. The temperature range of SXE is 75 to
375 degF [23 to 191 degC].

23. Which of the following systems are most

used for carbonate acidizing?
A. DAD, SXE
B. HCl
C. mud acid, clay acid
D. none of the above
24. Which of the following systems are most

used for sandstone acidizing?
A. DAD, SXE
B. HCl
C. mud acid, clay acid
25. What is mud acid?

A. a mixture of clay acid and acetic acid
B. a mixture of inhibited HCl acid and
hydrofluoric acid.
C. a mixture that can not only dissolve the
minerals that HCl acid can dissolve,
but can also dissolve siliceous
minerals presented in most sandstone
formations.
D. b and c
E. none of the above
26. What does DAD stand for?

A. diluted acid dispersion
B. dynamic acid dispersion
C. diffusion additives dispersion


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JET Manual 38

Copyright © 2007 Schlumberger, Unpublished work. All rights reserved.

Trademarks & service marks

An asterisk (*) is used throughout this document to designate a mark of Schlumberger.

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | iii

The fracturing fluid is a critical component of

1.1 Learning objectives

• Perform water analyses.

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 5

All employees working in fracturing laboratory ○ Rubber or plastic protective aprons

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 7

• Wellsite execution requirements

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 9

Figure 3-1. Field Laboratory Truck

Mud balance Digital titrator

Water bath Retort kit

Field QA/QC kit

Figure 3-2. Field QA/QC Kit

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 11

The laboratory technician (Fig. 3-3)

• works under the direction of the job

Figure 3-3. Laboratory Technician Hard at Work

12 | Laboratory Truck and Technician

The following are QA tasks that will need to

4.1.1 Iron concentration test

STEP 01 Insert the iron color disk into the

STEP 02 Fill a clean color test tube to the

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 13

• Throughout the job, linear gel should

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 15

Several tests are commonly performed at the 5.1.1.1 pH

• SG bottle For a more accurate reading, a pH meter

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 17

5.1.1.2 Specific gravity

STEP 01 Fill a graduated cylinder with the

18 | Typical Laboratory Tests

To calculate the SG of the sample water, use

STEP 01 Switch on the HACH2000

Figure 5-1. HACH2000 Spectrophotometer

STEP 02 Adjust the wavelength to 450 nm

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 19

STEP 01 Add 3 drops of phenolphthalein

indicator. P<1/2T T-2P 2P None

20 | Typical Laboratory Tests

5.1.4 Calcium and magnesium

1.020 and over 1 mL

STEP 02 Dilute to 50 mL with distilled

STEP 03 Add 3 to 4 drops of potassium

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 21

STEP 04 Add 2 scoops of Calver II STEP 03 Add 3 to 4 drops NH4OH.

For EDTA concentrations other than 0.025 M,

22 | Typical Laboratory Tests

STEP 06 Perform the following calculation: STEP 03

5.1.5 Sulphate, barium, iron, and STEP 07 Press SHIFT TIMER.

• BariVer® 4 Reagent Powder Pillow for

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 23

24 | Typical Laboratory Tests

JET 38 - WPS-Basic Laboratory Training and Fluid QA/QC | 25

• Allow gel to hydrate for an additional 10 min

26 | Typical Laboratory Tests