Dewatering Procedures PDF

Section 9 : Dewatering Procedures
Dewatering Manual v 1.0 131


9. Dewatering Procedures
The development of a clearly defined dewatering program for a particular project is essential to
the success of the project. The program cannot be written in isolation, but must take into
consideration a wide range of well site services, equipment and environmental regulations :
1. Well location : On- or off-shore, remoteness,
2. Rig Capability : Space and storage facilities, layout of rig and mud systems.
3. Well depth, trajectory and hole sizes,
4. Drilling Parameters : well bore stability, temperature and pressure,
5. Drilling Fluid types and properties,
6. Solids control equipment,
7. Environmental Regulations,
8. Re-cycled fluid compatibility.
At the rig site, the operator’s representative, rig manager, rig crew and the drilling fluid engineer,
must be aware of the objectives of the dewatering operation, along with the changes to normal rig
site practices and potential problems. The dewatering program must also outline flow rates, hole
sizes, solids control requirements, site layout diagrams, and chemical treatment programs
matched to fluid types. In addition expected equipment performance targets should also be
clearly stated, and in particular itemize the cost and logistical benefits to be derived from the
service.
9.1 Selecting the Most Efficient Dewatering Additives

If a fluid or mud type has not been dewatered previously, it is not a simple process to choose the
most appropriate coagulants or flocculants. There is a wide range of coagulants available, and an
even wider range of polymeric flocculants. Because of the number available and their proprietary
nature, it is difficult to select the best polymer for a specific task or type of drilling fluid.
Sections 3 and 4 describe the types of coagulants and flocculants and the mechanisms and
chemistry involved in their application. In addition, section 6 describes the processes involved
along with the mechanical components of dewatering systems. In order to effectively dewater any
particular fluid that may be encountered at the rig site, it is essential to have a working knowledge
not only of which are the most appropriate additives to use, but also the correct method of
application, and utilization of equipment. A brief overview of the dewatering process follows,
however, for a full description refer to the relevant sections.
9.1.1 Summary of the Dewatering process

Dewatering is the commonly used term used to describe the process of removing colloidal sized
particles from a fluid. However in reality dewatering is a phase separation process, which
employs, through the use of coagulants and flocculants, enhanced solids removal techniques.
Colloidal particles are generally less than 2 microns is diameter, and due to their small size
remain suspended in water or oil and will not settle out. In addition they cannot be removed
using conventional solids control equipment. The use of coagulants and flocculants causes the
colloidal particles to agglomerate or clump together and the formation of larger, denser particles
or aggregates, and enables them to be removed by conventional solids control equipment such as
the centrifuge.

In aqueous solution, colloidal particles are generally negatively charged, and they therefore repel
each other. This stabilizes the colloidal solution and prevents the particles from forming
aggregates. Coagulants and flocculants are used to destabilize the colloidal particles by removing
the negative charge, and also to increase the ability to agglomerate and form larger particles.
Coagulation and flocculation are separate processes, involving different mechanisms, and the use
of specific chemical additives.
9.1.2 Coagulation
Coagulation usually refers to the process of destabilizing colloidal particles by neutralizing the
negative charges on the colloidal particles, thus enabling them to aggregate and form small flocs.
Coagulants are typically cationic and are added using high speed mixers for quick and thorough
mixing. Flocs are formed almost instantaneously. Sufficient coagulant has to be mixed to ensure
that the charge on the colloidal particles is effectively neutralized. However over-treatment can
reverse the particle charge and redisperse it as a positive colloid. Therefore it is critical to ensure
that the correct dose is being employed.
There are two main groups of coagulants, inorganic metal salts and short chain cationic polymers.
Table 9.1 : Common Coagulants
Inorganic Coagulants Polymeric Coagulants
Aluminum sulfate Calcium sulfate PolyDADMAC
Ferric chloride Ca Ammonium Nitrate Epi-DMA
Ferric sulfate Calcium chloride Resin Amines
Ferrous sulfate Calcium nitrate
Polyaluminum chloride Potassium hydroxide
Calcium hydroxide Potassium chloride
a) The inorganic metal salts include multivalent compounds of calcium (Ca+2), magnesium
(Mg+2), aluminum (Al+3), and iron (Fe+2 or Fe+3). The coagulating power is highly dependent on
the valency or charge on the metal cation. A trivalent cation (+3) is 10 – 20 times more effective
than a divalent cation (+2), which is 30 – 60 times more effective than a monovalent cation (+1).
There are two main mechanisms by which inorganic salts achieve coagulation.
(i) Charge Neutralization. When sufficient metal cations such as Al+3 or Fe+3 have been
added to neutralize the negative charges, the colloidal particles become destabilized, and
agglomeration can occur.
(ii) Colloid Entrapment. At high excess concentration, the metal cations precipitate out as
hydroxide compounds, for example aluminum hydroxide and ferric hydroxide. The insoluble
hydroxide compounds can bridge together to form large complex particles which settle out.
The colloidal particles become enmeshed and drawn down with them in a process also
referred to as sweep flocculation.
Both mechanisms can be employed in the coagulation process, however colloid entrapment
generally gives better results. The main disadvantage of charge neutralization is that precise
control of dosage and pH are required for optimum coagulation. Over-treatment results in re-
stabilization of the colloid. The concentration of colloidal particles in a drilling fluid will
fluctuate constantly depending on the drilling parameters, formations being drilled and
operation of the solids control equipment, thus making precise control difficult.

Colloid Entrapment overcomes these problems. Using higher doses of coagulant, the
hydroxide precipitate forms rapidly, over a wider pH range, and produces larger and stronger
aggregates giving better particle removal.
Inorganic metal salts are pH dependent. Most are amphoteric, being soluble at both low or high
pH, but insoluble at intermediate pH. When dissolved in water to form the metal hydroxide the
pH must be adjusted to the point of least solubility of the hydroxide. At this point the metal
hydroxide precipitates, in some cases in the form of large complex particles and producing the
sweep floc. The pH range of least solubility is specific to the metal salt.
Table 9. 2 Optimum pH Range for Inorganic Coagulants

Inorganic Coagulant pH Range
Aluminum Sulfate (Alum) 6.5 – 7.5
Ferric Chloride 4 - 11
Ferric Sulfate 4 – 6, and 8.8 – 9.2
Ferrous Sulfate > 9.5
Adjustment of the fluid pH to produce a sweep floc is important for several reasons :
(i) Using the correct pH range for a particular inorganic coagulant ensures that the metal
hydroxide is insoluble and starts to precipitate out. The sweep floc formed then drops out
the colloidal particles.
(ii) The sweep floc also takes out with it any excess metal salts, minimizing carry over to the
effluent.
The polyvalent aluminum and iron metal salts are unique in that they produce large highly
cationic molecular hydroxide species in water, which rapidly form large dense sweep floc
aggregates. The divalent metal salts of calcium and magnesium react differently in water to
produce less dense precipitates of calcium carbonate. To initiate precipitation, some carbonate
alkalinity is required.
Table 9. 3 Advantages and Disadvantages of Inorganic Coagulants

ADVANTAGES DISADVANTAGES
Low cost pH adjustment is critical
Widely available (some commonly used in muds) Possible metal carry over in effluent
Not sensitive to over-treatment for sweep flocs High floc volume
May remove organics and heavy metals Adds solids (salts) to the system
Alum and ferric hydroxide flocs tend to be hydrated
and difficult to dewater
b) Polymeric Coagulants are low molecular weight polymers with very high cationic charge
density. Since charge neutralization is the only coagulation mechanism, over treatment will result
in re-stabilization of the colloid. However, the effective polymer dosage required may be as low
as one tenth that required for inorganic coagulants and therefore overdosing is less critical. They
require high shear mixing, and are often used in conjunction with other coagulants.

Table 9. 4 Advantages and Disadvantages of Polymeric Coagulants over Inorganic Coagulants
ADVANTAGES DISADVANTAGES
Lower Dose Level (up to 90% less) than inorganics Sensitive to incorrect dose. Over treatment
Lower floc volume (50 – 90% less) than inorganics destabilizes colloids
Flocs are more easily dewatered Effluent clarity is generally less. For NTU < 0.1
Not sensitive to pH inorganic coagulants may be required.
No additional solids Not suitable for removal of organics (mud polymers
No carry over of metals etc). which requires inorganic coagulants.
9.1.3 Flocculation
Flocculants are generally used as coagulant aids, and they are used after the addition of
coagulants. They are long chain, high molecular weight polymers, and act by bridging
coagulated particles to create larger flocked structures which become large enough to be removed
by a centrifuge.
The most common bridging polymers are polyacrylamides and are available in cationic, anionic
and non-ionic forms. A wide range of polymers are available, however the majority carry a
positive or negative charge to enable them to adsorb onto the particle surface by electrostatic
attraction. In water this charge also enables the polymer to uncoil due to charge repulsion along
its length. The important characteristics of polymer flocculants are charge type, charge density
and molecular weight:
(i) The charge type of Polymer refers to the overall charge on the polymer, i.e. cationic (+),
anionic (-), or non-ionic.
Non-ionic polymers have no readily ionizable groups, but most are slightly charged due to
impurities or partial hydrolysis in water. Most are polyacrylamides and have similar
properties to anionic polymers.
Anionic polymers ionize in water to give negatively charged areas on the polymer. Most are
copolymers of acrylic acid and acrylamide. They range from practically non-ionic to very
strongly anionic, and have a variety of charge densities, although the intermediate charge
densities are usually the most effective. They are the most widely used flocculants for clear
water drilling and dewatering situations, and are generally used with inorganic coagulants.
They are effective in treating most spud muds and bentonite systems
Cationic polymers are positively charged in water and have a wide range of families, charge
densities and molecular weights. Most are poorly ionized at neutral to alkaline pH, and
therefore pH adjustment is normally required. They are most commonly used to flocculate
salt muds, including seawater, KCl and NaCl systems, and are effective with low percentages
of oil.
(ii) Charge density is controlled by the ratio of charged and uncharged monomers in the
polymer chain. In general, the charge density of common anionic polymers is in the range of
0% – 40%, that for cationic polymers is 0% to 70%.
(iii) Molecular weight describes the overall size of the polymer and most flocculating
polymers are in the range of high to very high molecular weight (>10,000,000). The
molecular weight is only a measure of the average polymer length, as the polymer chain

length varies. Manufacturers use different methods to measure the chain length. Therefore,
polymers listed as equivalents, may actually be quite different. In general, flocculating power
increases with molecular weight.
(iv) Molecular structure. Polymer chains may be linear or highly branched. The more
linear the polymer, the more particles that it can adsorb and bridge.
Figure 9.1. Polymers and Flocculation Applications

Drying beds
Dewatering Paper Sludge
Dewatering Drilling Mud Paper effluents

’Iron mud’
Flocculants Dewatering Primary Sludge
Dewatering Secondary Sludge
Dewatering Alkaline Sludge

Clarifying Industrial
Coal Washing
Effluent
Dewatering
Clarifying Industrial Effluents Digested Sludge
Dewatering
Paper retention aids Biological Sludge
Sugar applications Raw Water Clarification and

Oily Waste
Color Removal
100% 50% 0% 50% 100%

very high high low medium high
ANIONIC NONIONIC CATIONIC
Adapted from D.A. Mortimer (1991) Polymer Int. 25, 29-41
Polymers are supplied in three main forms, dry powder, liquid and emulsion polymers. Dry
powders require premixing to dissolve the polymer and allow the chains to uncoil. Emulsion
polymers also need premixing to activate the polymers. Due to the very high viscosity of the high
molecular weight polymers in water, there is a limit to molecular weight in the liquid polymer
form. Emulsion polymers overcome this limit by emulsifying the water soluble polymers in
droplets of water dispersed in oil.
9.1.4 Factors Effecting Coagulation and Flocculation

A large number of factors influence the effectiveness of the dewatering process. The correct
choice and dose of coagulant or flocculant is critical and will require laboratory tests prior to the
job, as well as regular pilot tests at the rig site.
Preliminary bench testing of polymers is an important part of the selection process, even when the
polymer is used as a flocculant aid for an inorganic coagulant. Adding an untested polymer
without knowing the optimum dosage, feed concentration or mixing requirements can cause poor
results. It is important to note that, within the same family or type of polymer, there can be a large
difference in molecular weight and charge density. For a specific application, one member of a
family can have just the right combination of properties and greatly outperform the others.
If tests need to be run before the job, it is important to obtain samples of the make up water and
mud products. Variations in these from what will be used at the rig site may result in the wrong
choice of coagulants or flocculants. These tests will also determine if pH adjustment is
necessary.

Table 9.5 : Factors Effecting Coagulation and Flocculation
Influencing Factor Coagulation Flocculation

Dosage Use excess for sweep flocs Pilot test to avoid excess
Mixing Energy Rapid high shear mixing Low shear mixing
Contact time Coagulation is instantaneous Polymers need time to adsorb onto and
bridge solids
pH pH adjustment normally required pH adjustment may be required
Solids concentration Use barite recovery in weighted muds. Use barite recovery in weighted muds.
Dilute solids to <5% Dilute solids to <5%
Viscosity Dilute further in high viscosity fluids Dilute further in high viscosity fluids to
to allow flocs to form. allow flocs to form.
9.2 Pilot Testing Procedures

Pilot testing should be carried out in the M-I SWACO lab prior to the start of a project. This is
especially important if the drilling fluid system to be used does not have a history of being
dewatered, and will ensure new additives and systems are capable of being dewatered and
determine the treatment and chemical selection required. On location, the Dewatering Engineer
should be equipped with a dewatering pilot test kit containing a wide range of coagulants,
flocculants, buffers, acids and bases to run routine pilot tests and troubleshooting programs.
The objective of pilot testing is to determine the most effective and economical chemical
treatment for a given fluid system. The economics will be based on the number of chemicals and
concentration of each required in order that satisfactory results are obtained. The effectiveness of
various chemicals is subjective, based on the size (larger is better than small) and stability
(durable is better than fragile) of the flocs and the clarity of the resultant liquid. Most fluids that
require dewatering are stable suspensions of solids in liquids. This stability refers to the tendency
of the fluid to remain homogeneous over a period of time as opposed to separating into layers of
solids and liquid. This stability often is desirable while the fluid is used for its intended purpose
but requires added effort for the separation process.
It is essential when carrying out pilot tests, to properly document the results obtained. It is likely
that a wide range of tests will need to be carried out, and proper documentation will avoid
duplication of tests, and enable recognition of trends.
9.3 The Jar Test

The most commonly used bench test is the Jar Test. With simple modifications it provides the
quickest and most economical method to obtain reliable data on variables that affect the
dewatering and treatment process and design parameters. The principle involved is flocculation
of the colloidal particles causing turbidity, and clarification of the fluids that have been given
specific treatments.
The jar test involves mixing the fluid to be tested in a glass or clear plastic jar, with water and
dewatering products. The method can be quick and “dirty”, using “bucket” chemistry methods to
quickly screen a large range of products in a short time. This can then be followed by more
precise methods to determine more accurate additions.

Figure 9.2. Flocculation of Drilling Fluids and Clarity of Supernatant Liquids
The design and dimensions of the “jar” will be dependent on the test conditions and apparatus
used, and can vary from open topped glass or clear plastic beakers, to glass or clear plastic jars
with caps to allow for mixing by hand. The most important variables in the jar test are the actual
test procedures used to perform the evaluation of the coagulants and flocculants. Proper
procedures will provide good and meaningful results. The tests carried out should be properly
documented to avoid duplication and misinterpretation of results. An important rule in running
jar tests is that only one variable should be assessed in each test run, i.e. only one variable should
be changed through a series of tests. For example, the dosage of a particular coagulant added.
The following applications for jar testing may be more important than its use in routine dosage
control. It is studies such as these where the jar test has its major value, since the results are worth
the time and effort to do the test properly:
1. Dilution required to promote flocculation.
2. Dispersion of coagulant, polymers and other reagents
a. selection of primary coagulant or coagulants.
b. effect of pH on the treatment process.
c. optimum dosages of the coagulants, polymers and pH modifiers.
d. mixing energy and mixing time studies (rapid mix)
e. effect of coagulant and polymer application, means and method, including dilution.
f. optimum timing and sequence of application of the chemicals.
g. optimum feed point for pH adjusting chemicals.
Figure 9.3. Jar test Apparatus
The jar test apparatus shown in Figure 9.3 is a specially designed apparatus to test up to 6 fluids
simultaneously.

9.4 Equipment and laboratory space.
The following equipment is required for bench-scale laboratory testing:
(i) Jar Test Stirring apparatus (Fig 9.3) with variable speed control to about 150 rpm and with
provision for six 2-litre beakers. A direct, positive, mechanical drive is recommended.
(ii) Turbidimeter (light scatter type) of range about 0.01-1,000 NTU.
(iii) pH meter.
(iv) At least six 2-litre jars
(v) Miscellaneous glassware or plastic ware for holding samples, mixing reagents, making
dilutions, etc. The lower risk of breaking high quality plastic ware may be important.
(vi) Pipettes/syringes of 1 ml, 5 ml, 10 ml, 25 ml and 100 ml capacity.
(vii) Graduated beakers or flasks of 10 ml, 25 ml, 100 ml, 500 ml and 1,000 ml capacity.
(viii) Stopwatch with a sweep second hand.
(ix) Inorganic Coagulants. Stock at least : Lime, Calcium Sulfate (Gyp), Calcium
Ammonium Nitrate, 10 % Al2(SO4)3 and 10 % FeCl3 stock solutions.
(x) Cationic, anionic and non-ionic polymers. Make up polymer stock solution from dry
reagent at 0.5% concentration.
(xi) Distilled water.
(xii) Raw water.
(xiii) Lime solution, 1 per cent. Made up daily (may use another reagent for alkalinity).
(xiv) Magnetic stirrer and stirrer bar.
(xv) Hamilton Beach Mixer or equivalent.
Note : Ensure that all glassware etc is properly cleaned between tests to prevent cross
contamination. Many of the polymers used are extremely difficult to remove.
9.5 Testing in the Laboratory.
9.5.1 Preparation
Prior to starting the series of tests, the fluids to be tested, and the working solutions of coagulants
and flocculants need to be prepared.
(i) Homogenize the mud sample to be tested in a Hamilton Beach Mixer or equivalent for 30
minutes. If the mud is not a field sample and is to be mixed from scratch, allow adequate time to
premix the fluid and for products to yield If possible only use samples of products, and make up
water, that will be used locally.
(ii) Prepare fresh working solutions of the coagulants and flocculants.
9.5.2 Dilute the Test Fluid

Inadequate dilution is one of the main reasons that dewatering fails at the rig site. Extensive
dilution is often seen as being in conflict with the concept of reducing waste fluids at the rig site,
however it is a necessary and essential step. In most cases a 50% dilution will be not be sufficient
to effectively dewater a drilling fluid. It will probably be necessary to increase the dilution to 70
or 80%, depending on the viscosity and level of solids in the fluid. Therefore, to carry out the
initial tests, dilute the test mud by 80%, i.e. 80% water/20% mud.
Dilution is necessary because the flocs, once formed, need to be visualized. If the solids are too
close together they can not be seen and are unable to settle. Also dilution reduces the viscosity of

the fluid to aid in floc settling. If the fluid is not diluted sufficiently, the tests will either fail, or
produce poor results and require unnecessary over-treatment with expensive polymers. In the
testing phase, it is better to over-dilute than under-dilute. With over-dilution, a good result will
almost certainly be achieved faster. If necessary, the tests can then be repeated with lower
dilution levels to determine optimum conditions.
In most cases however high dilution will be required. It is a necessary and essential step in the
process of dewatering and does not conflict with the concept of reducing waste fluids. The
dewatered fluid can be used for dilution or to make new mud, or be recycled through the
dewatering process as dilution fluid, this minimizing the increase in fluid volumes at the rig site.
9.5.3 Choice of Working Solution Concentrations

The amount and concentration of coagulant or flocculant to add to the diluted fluid sample will be
dependent on the volume of the sample. In general, the required treatment for coagulants is in the
range of 500 – 5,000ppm and may be as high as 10,000ppm for weighted, highly dispersed or
KCl PHPA systems. For most flocculants the required range is from 200 – 1,500ppm. Therefore
it is important to ensure that the dose delivered is within range and does not cause over-treatment
if too concentrated, or has to be added in large volumes because it is too dilute.
1ppm = 1g/m3 = 1mg/l
Therefore for various concentrations of solutions:
a) A 10% by weight solution contains 10g chemical in 100g solution (100ml) or,
10 parts in 100 = 100,000ppm, 100g/l, 100kg/m3, or 100mg/ml.
b) A 1% solution contains 1g chemical in 100g solution (100ml) or,
1 part in 100 = 10,000ppm, 10g/l, 10kg/m3, or 10mg/ml.
c) A 0.2% solution contains 0.2g chemical in 100g solution (100ml) or,
0.2 part in 100 = 2,000ppm, 2g/l, 2kg/m3, or 2mg/ml.
Table 9.6 Effect of sample size and working solution strength on final sample concentration
Working Solution Dosage Delivered Final concentration in sample per 1ml addition
(% by wt.) (mg/ml) 200ml Sample 20ml sample
10 100 500ppm or 500mg/l 5,000ppm or 5,000mg/l
1 10 50ppm or 50mg/l 500ppm or 500mg/l
0.2 2 10ppm or 10mg/l 100ppm or 100mg/l
In the examples in Table 9.6, the coagulants and flocculants were added to 200ml or 20ml
samples of diluted mud. Using the same concentration of chemicals for both samples may not be
appropriate. A 10% solution of coagulant may be used in a 200ml sample if each 1ml addition
increases its concentration by 500ppm and the desired range is 500 – 5,000ppm. However, with
the smaller 20ml sample each 1ml addition will increase the concentration of the coagulant by
5,000ppm resulting in potential over treatment and erroneous results. In this case a 1% solution of
coagulant would be more appropriate.
Similarly, a 1ml addition of 1% flocculant solution in a 200ml fluid sample will increase the
concentration of the flocculant by 50ppm, and in a 20ml sample by 500ppm. Therefore the 1%
solution is acceptable for the 200ml sample but not for the 20ml sample, where a 0.2% solution
would be more appropriate.

9.5.4 Determine the Optimum Coagulant Dose
The testing program usually begins with determination of the optimum coagulant dose. As with
any laboratory work, all containers should be labeled explicitly and each measurement or action
should be recorded on paper as it is taken, otherwise whole test runs may have to be repeated for
the sake of small interruptions such as a telephone call. The procedure is as follows:
(i) Add the fluid to the jar and dilute with water. Never completely fill the jars. The starting
volume should be around one half to two thirds of the jar capacity. This allows room for proper
mixing, and for additional dosages to be added. For a 2 liter jar, and for a final fluid volume of 1
liter, add 800 ml water to 200 ml mud, and incremental doses of coagulant (Table 9.7).
Note : Jar 1 is used as a control, i.e. no treatment for comparison purposes.
Table 9.7 : Example Testing Program for Coagulant Dose.
Jar 1 Jar 2 Jar 3 Jar 4 Jar 4 Jar 6
(Control)
Mud (ml) 200 200 200 200 200 200
Water (ml) 800 800 800 800 800 800
0.1% Coagulant (ml) 0 10 20 40 60 80
Coagulant (mg/l) 0 10 20 40 60 80
pH Measure Measure Measure Measure Measure Measure
(ii) Mix at 100 rpm for 2 minutes. Coagulants, such as metallic salts, help cause smaller
aggregates to form larger particles. Then stop the mixer and observe each jar for formation
of pinhole flocs. Measure the pH of each solution.
(iii) If flocs have formed, choose the optimum case and proceed to the next stage.
(iv) If flocs have not formed, make pH adjustments to each jar with acid and alkali to vary the
ph between 4 and 12.
(v) If flocs have still not formed after pH adjustment, repeat the tests using another coagulant.
(vi) Document the results.
9.5.5 Determine the Optimum Flocculant Polymer Dose.

In most cases a flocculant polymer is required in addition to the coagulant. Low molecular weight
cationic polymers act as coagulants and are used to supplement the coagulant dose. In some cases
a small dose of cationic polymer during the initial mixing can significantly reduce the required
amount of primary coagulant. In addition to the quantity of polymer, the sequence of coagulant
and polymer addition may be important, and tests will show which should be added first. In some
cases the polymer may form satisfactory flocs on its own.
High molecular weight cationic, nonionic and anionic polymers increase the agglomeration of
flocs for settling. In this case the polymer must be applied after the floc has formed, otherwise it
will be less effective. If applied too late there may not be enough time remaining for optimum
floc formation. It is therefore important to test carefully when in the flocculation process to add
such polymers. Experience suggests the best time is about 5 minutes after beginning the
flocculation cycle.
When evaluating polymers, the same general procedure and mixing regime is followed as for
coagulants, using the coagulant dose that was previously selected. The stage at which polymer is
applied will depend on the objectives and polymer type. They should be added as a very dilute
solution (at most 0.2%), because low concentrations are required.

(i) Add the fluid to the jar and dilute with water. Never completely fill the jars. The starting
volume should be around one half to two thirds of the jar capacity. This allows room for proper
mixing, and for additional dosages to be added. For a 2 liter jar, and for a final fluid volume of 1
liter, add 800 ml water to 200 ml mud, the optimal dose of coagulant and pH, and incremental
doses of flocculant polymer (Table 9.8).
Note : Jar 1 is used as a control, i.e no treatment for comparison purposes.
Table 9.8 : Example Testing Program for Flocculant Dose.

Jar 1 Jar 2 Jar 3 Jar 4 Jar 4 Jar 6
(Control)
Mud (ml) 200 200 200 200 200 200
Water (ml) 800 800 800 800 800 800
Coagulant (mg/l) Optimal Optimal Optimal Optimal Optimal Optimal
pH Optimal Optimal Optimal Optimal Optimal Optimal
0.1% Flocculant Polymer (ml) 0 10 20 40 80 160
Flocculant Polymer(mg/l) 0 10 20 40 80 160
(ii) Add the optimal dose of coagulant, and adjust the pH as necessary for optimal coagulation.
Mix at 100 rpm for 2 minutes.
(iii) Add the flocculant polymer and mix at 20 rpm for 15 minutes. The slower mixing speed
helps promote floc formation by enhancing particle collisions which lead to larger flocs and also
prevents shearing the flocs due to turbulence. Then stop the mixer and observe each jar for
formation of bulky tight flocs that rapidly settle out.
(iv) If good tight bulky flocs have formed, allow the jar to stand for 30 minutes to determine how
well the flocs settle.
(v) Evaluate the turbidity of the supernatant fluid roughly by sight or more accurately using a
nephelometer.
(vi) If flocs have not formed, repeat the tests using another flocculant.
(vii) Document the results.
9.5.6 Fine Tuning the Optimum Doses and Dilution Requirement.

It is assumed that the tests carried out so far have identified at least one successful treatment
process. That process can be further fine tuned by repeating the dose runs using doses close to
that which gave the best result. For example in section 9.5.3, if the optimal dose of coagulant was
60 mg/l, carry out a series of tests where the dose is varied between 45 and 75mg/l. Repeat with
the flocculant additions.
Lastly the dilution tests can be re-run to determine the optimum dilution requirement that will still
allow flocculation to occur efficiently.
9.6 Field Testing

Pilot tests should be carried out routinely at the rig site to confirm correct treatment and that the
treatment is optimized. Even if the process is routine, and has been used successfully with the
same mud systems, it is still necessary to confirm correct treatment. In the field there are several
possible scenarios which need to be taken into consideration:
(i) The fluid or fluids to be dewatered have been successfully dewatered in the same area before.
In this case the coagulants and flocculants required will be well known. However pilot tests

should still be carried out to determine the effect of make up water, and any minor adjustments to
the equipment set up, mixing times and so on. If there are any major differences, such as make
up water, formations drilled, pre-job testing should be carried out in the district lab. If possible,
any fluid dilutions carried out in the district lab, should be done with the make up water to be
used at the rig site.
(ii) The fluid or fluids to be dewatered have been successfully dewatered in a different area
before. In this case the range of coagulants and flocculants that are successful with the system or
systems will be known. As the product mix or sources may differ, it is imperative to carry out
pre-job testing in the district lab. Samples of mud products and the make up water to be used at
the rig site should be used for the fluid make up. The results should then be confirmed at the rig
site.
(iii) The fluid or fluids to be dewatered have not been dewatered before. In this case, the range of
coagulants and flocculants that will be successful will not be known. Therefore it is essential that
pre-job tests are carried out in the district lab along with support from the technical services
laboratory in Houston. Extensive testing may be required to determine the products required.
Again samples of mud products and the make up water should be used for the laboratory tests,
and the results confirmed at the rig site.
9.7 Field Testing - The Quick and “Dirty”, “Bucket” Chemistry Method
Quick and “dirty” tests can be carried out with the minimum of equipment and should be used for
screening purposes only.
Equipment required:
1. Range of Coagulants and Flocculants to be tested (Field Test Kit).
Polymers should be pre-prepared at working solution strength.
2. 300 ml clear glass or plastic graduated beakers.
3. Magnetic stirrer and stirrer bar (to mix polymers).
4. Plastic Dropper Bottles for storage of stock solutions.
5. Range of disposable syringes
6. Spatula
A. Selection of Coagulant.
(i) Add approximately 160 ml water to beaker. Add inorganic coagulant to the water and mix.
(ii) Add approximately 40 ml mud and stir vigorously with a spatula.
(iii) Stop stirring and observe for pin flocs
(iv) Add further coagulant if required.
(v) If pin flocs occur, try pH adjustment to determine the effect (more or less flocs formed).
(vi) Repeat with alternative coagulants as necessary.
B. Selection of Flocculant.
(i) Repeat preparation of the diluted mud with the coagulants that produced the best pin flocs.
(ii) Add increasing amounts of the flocculant and stir slowly until bulky tight flocs are formed.
(iii) If no flocs form, repeat tests with other flocculants. Try a ranges of polymer from low to
high charge density, and varying charge (cationic, anionic, non-ionic)
Based on the results obtained, and assuming that good results were obtained for at least one
combination of coagulant and flocculant, repeat tests can be run to fine tune the mixing and doses

of the products. The tests can also be carried out as in the Field Pilot Tests (Section 9.4), or by
using the specially developed Jar Test Apparatus
9.8 Standard Field Test Procedures

9.8.1 Step 1: Dilution of Mud Sample
As described in previous test procedures, adequate dilution of the test fluid is essential. The level
of dilution required is dependent on the level of solids in the fluid. Some muds may require 70 –
80% dilution. If other waste fluids, containing lower levels of solids, will be dewatered at the rig
site then lower levels of dilution will be required.
A good starting point for most muds is an 80% dilution (80% water/20% mud).
1. Add 40 ml. of drilling fluid to be flocculated to a glass vessel.
2. Add 160 ml of make up water to the glass vessel. Invert glass vessel several times to insure a
homogeneous mixture.
3. Note the pH of the resultant solution.
9.8.2 Step 2 : Choice of Working Solution Concentrations

The amount and concentration of coagulant or flocculant to add to the diluted fluid sample will be
dependent on the volume of the fluid sample to be tested. This is discussed in section 9.5.4. In
general, the required treatment for coagulants is in the range of 500 – 5,000ppm and may be as
high as 10,000ppm for weighted, highly dispersed or KCl PHPA systems. For most flocculants
the required range is from 200 – 1,500ppm. Therefore it is important to ensure that the dose
delivered is within range and does not cause over-treatment if too concentrated, or has to be
added in large volumes because it is too dilute.
At this point a prepared solution of 1% flocculant can be added to determine if a pH adjustment is
not needed. Normally the only drilling fluids which do not need pH adjustment for flocculation
are fluids that are contaminated with cement and salt muds (Over 60,000 TDS).
In some cases, adjustment of pH is critical to the coagulation process. The optimal pH is
determined by a number of factors, such as the type of drilling fluid, but generally the pH
requirement is controlled by the type of coagulant being used, e.g. aluminum sulfate works best at
pH 6.8 – 7.5, ferric sulfate and ferric chloride at pH 8 – 10, and lime at pH 10 – 12.
9.8.2 Step 3: Determine if pH Adjustment Needed

1. Add 1 ml. of prepared 1% flocculant solution to the 200 ml diluted drilling fluid sample.
2. Invert vessel 5 times and observe for flocculation. Do not shake the bottle.
3. Each 1 ml addition is equal to 10mg of flocculant (50 ppm or 50mg/l diluted mud). In general
the concentration range for flocculants is 100 – 1,500ppm.
4. Continue to make additions of flocculant. Invert after each addition and observe for
flocculation.
5. Once flocculation is observed note volume (ml) of flocculant solution used.
6. Continue to make additions of flocculant and observe floc quality and size.
7. Observe shear stability of floc by shaking bottle vigorously for 5 seconds. Add additional
flocculant and observe to see if flocs will reform.
8. Pilot test different flocculants, anionic, cationic and nonionic, to determine best overall.

9. If no flocculation occurs proceed to next step.
9.8.3 Step 4: pH Adjustment

Adjustment of pH is normally needed to maximize the flocculation mechanism. Make sure that
the type of acid or alkali in the pilot test kit is the same as that to be used on the rig.
1. Add acid/alkali drop by drop to the diluted drilling fluid sample.
2. Check the pH with either the strips or pH meter.
3. Make visual observation of fluid. Additions of acid or alkali may form small pin flocs, which
are an indication that coagulation is taking place.
4. After addition of acid/alkali is made flocculation can be attempted once again.
9.8.4 Step 5: Flocculation of pH Adjusted Drilling Fluid Sample

1. Add 1 ml. of prepared 1% flocculant solution to the 200ml drilling fluid sample.
2. Invert bottle 5 times and observe for flocculation. Do not shake bottle.
3. Each 1 ml. addition is equal to 10mg of flocculant (50ppm or 50mg/l diluted mud). A typical
lightly dispersed 9 lb/gal drilling fluid requires 300 - 600 ppm flocculant.
4. Continue to add flocculant. Invert after each addition and observe for flocculation.
5. Check pH of fluid to insure that the pH is still 7.
6. Once flocculation is observed note number of ml. of flocculant solution used.
7. Continue to make additions of flocculant and observe floc quality and size.
8. Observe shear stability of floc by shaking bottle vigorously for 5 seconds. Add additional
flocculant and observe to see if floc will reform.
9. Pilot test different flocculants (anionic, cationic, nonionic) to determine best overall.
10. If flocculation does not occur with a pH adjustment the fluid will require the addition of a
coagulant. Typically fluids that are highly dispersed with lignosulfonates or polymeric
thinners will require the addition of coagulants.
9.8.5 Step 6: Flocculation of Drilling Fluid Which Requires Coagulation

1. Add acid drop by drop to the 200ml diluted drilling fluid sample.
2. Check the pH with either strip or pH meter.
3. Add acid until pH 7.
4. Inorganic Coagulant with a 10% solution
5. Add 2-3ml of prepared 10% inorganic coagulant solution.
6. Each 1ml of 10% inorganic coagulant is equal to 100mg coagulant (500ppm or 500mg/l
diluted mud). Typically additions of 500 to 10,000 ppm of coagulant may be required. If
large additions are needed it may be necessary to evaluate the cost efficiency of the
coagulant.
7. Go to 11.
8. Organic Coagulant with a 1% solution
9. Add 2-5 ml prepared 1% organic coagulant solution.
10. Each 1 ml of 1% organic coagulant is equal to 10mg of coagulant (50ppm or 50g/l diluted
mud. Typically additions of 500 to 10,000 ppm of coagulant may be required.
11. If no flocs appear repeat Step 5 with alternative coagulants.
If large quick settling flocs form, then further addition of flocculants may not be required.
If pin-hole or small flocs appear, addition of flocculants may be required. Go back to Step 5.

9.9 Preparation of Coagulant and Flocculant Stock Solutions
The preparation of stock solutions for evaluation purposes is a vital part of the testing procedures.
In general the coagulants and flocculants are diluted for test work for three reasons, ease of
handling, to ensure good mixing and, in the case of flocculants, to allow for activation.
A range of coagulants and flocculants will be supplied with the field pilot test kits. The method of
dilution will depend on the type of product. It is important to have the MSDS and product data
sheets. These provide information relating to type of charge, charge density, molecular weight
range, % active solids, specific gravity, dissolution time and viscosity, which will be needed to
determine the appropriate dilution procedures.
Dilution of the coagulant or flocculant chemicals is generally completed in 3 stages:
1. First dilution stage. This is termed the primary make-up. A small amount of chemical is
mixed into a prescribed volume of distilled water to form the stock solution. Most stock
solutions range from 0.5% (0.5 g/l) to 1.0% (10 g/l), and should be stored away from direct
sunlight and disposed of within 7 days for anionic flocculants, and 3 days for cationics.
2. Second dilution stage. This is termed the secondary make-up. The stock solution is further
diluted to form the working solution. A small amount of stock solution is mixed into a
prescribed volume of water, generally the water used at the rig site. Recommended working
solution strengths are 0.05% (0.5 g/L) for low solids slurries, to 0.2% (2 g/L) for high solids
slurries. Working solutions should be disposed of after 24 hours from the time of
preparation, and therefore should be clearly labeled.
3. Third dilution stage. In this final step, the working solution is added to the test slurry itself.
A small portion or dose of the working solution is added to a prescribed volume of the slurry
for analysis in a jar or other test. The final concentration of coagulant or flocculant chemical
is the same as that concentration that would be added to the slurry in the flocculation unit.
9.9.1 Recommended Pilot Testing Equipment required:

1) 1.0ml Disposable syringes
4) Stir Bar (1.75”)
5) Plastic Beakers, 400ml
6) Magnetic Stirrer, 1500 rpm (2 PREFERABLY)
7) Pocket Balance, 0 to 250 gram (0.1g readability)
8) 1 Liter Acrylic Cylinders with Stoppers
9) Graduated Cylinder, 250ml
10) Graduated Cylinder, 1000ml
11) Stainless Steel Rack
12) 4 oz. LDPE Narrow Mouth Bottles
13) 8 oz. LDPE Narrow Mouth Bottles
14) Bottle Brush
9.9.2 Preparation of Inorganic Coagulants.

For products such as alum, PACl, ferric and ferrous salts, and the simple solution cationic
polymers, simple dilutions can be made. Solution strength or active content and specific gravity

(S.G.) should always be factored into the dilution calculations. The coagulant concentrations
used can range from 0.5% to 5% by weight. In general a 1% solution is recommended to allow
for accurate delivery, good mixing and reasonable volumes to handle.
Stock Solution Preparation. A 10% solution is defined as 10% by weight, i.e. 10g (or 10,000
mg) of chemical in 90g (or 90ml) water, for a total of 100g. 1 ml of this 10% solution will
contain 100mg of chemical, (1ml = 1/100 x 10,000 mg = 100 mg).
Working Solution preparation. A 1% solution is prepared by adding 10ml of stock solution to
90ml of water, to give 1g of chemical in 100g solution.
1. Polyhydroxy Aluminum Chloride (PACl). To prepare 1% stock solution of PACl, the S.G.
must be known. 18% PACl has an S.G. of 1.37, therefore 1 ml will weigh 1.37 g.
1g = 1/1.37 ml = 0.73 ml (weight = volume/density)
Therefore 1% PACl can be prepared by adding 0.73 ml neat PACl to 99 ml water.
2. Aluminum Sulfate. To prepare a 1% solution of alum (dry basis) both the S.G. and solids
content must be known. Typically alum has an S.G. of 1.34 and a solids content of 48.5%.
1g alum solution = 1/1.34 ml = 0.746 ml
However since alum is 48.5% active, 1g of solution will only contain 0.485 g alum.
Therefore, 1g alum = 0.746 x 1/0.485 = 1.54 ml
1% alum (dry basis) is prepared by adding 1.54 ml liquid alum (48.5%) to 99 ml of water.
9.9.3 Preparation of Powder or Granular Polymer

When preparing stock solutions from products in granular form, the formation of lumps or “fish
eyes” should be avoided as it will result in incomplete dissolution and inaccurate dosages. It is
important for each granule to be wetted by the water.
To facilitate this, stir vigorously using a finger-type, anchor-type or magnetic stirrer to form a
light conical vortex. Add the granules so that they fall singly into the water and are drawn into
the vortex. Then reduce the mixing speed to remove the turbulence, but keeping the particles in
motion. The particles swell as the polymer hydrates and uncoils, and the solution becomes more
viscous. The polymer will be fully dissolved after 60 minutes and ready to be further diluted for
the working solution.
If distilled water is used to prepare the stock solutions, they may remain usable in a sealed bottle
for up to 2 months. Ensure that the bottle is properly labeled and with the date of mixing.
Preparing a 0.5% stock solution

This method uses a calculation by weight. Note that most polymers are between 92 and 98
percent pure. The example below uses 95% purity.
Weight of polymer (g) = (W x 1000 x L)
P
Where: W = Percent by weight of polymer solution desired, e.g. 0.5%
L = Total volume of solution being prepared (Liters). For 250 ml = 0.250L

P = (%) Percent Activity of the polymer (MSDS or Product Data Sheet).
Example: Determine the volume of powder polymer needed to prepare a 250 ml stock solution
containing 5.0 g/l (0.5% solution) of polymer by weight. Example has a 95.0% percent activity
using ABC Type Polymer.
Weight of polymer (g) = (0.5 x 1000 x (250/1000) = 1.32 g
95.0
Result: Add 248.68 ml water to a plastic beaker and insert a magnetic stir bar. Adjust the rpm on
the magnetic stirrer to develop a large/strong vortex. Weigh out 1.32 grams of sample and add
slowly along the sides of the vortex. Reduce the turbulence and allow to mix and hydrate for
approximately 60 minutes.
Note : The dissolution of the polymer may be improved by adding 2 ml of acetone to the powder,
prior to the addition of water.
Designate a number, or letter, to each of bottle containing a working polymer solution.
Example: ABC Type Polymer, 0.5% solution = Polymer Sample #1. Include date/time of blend.
9.9.4 High Molecular Weight Liquid Solution Polymers and Emulsion Polymers
The following procedures apply to Mannich polymers, polyamines, polyDADMACs, poly-
acrylamides, etc. With high molecular weight emulsion polymers, dilution before use serves two
purposes, activation of the chemical and accurate delivery during evaluation.
Stock solutions of emulsion polymers can be prepared in the same way as for granular products.
Pour the emulsion slowly in a thin stream into the conical vortex created by the mixer. Allow 20
minutes for complete dissolution of the emulsion polymer.
Stock solutions of liquid solution polymers have a very short dissolution time and can be made by
simply pouring them into water while stirring.
Preparing a stock solution

A 1% solution is acceptable for coagulants or solution polymers, but is not practical for emulsion
polymer as the solutions would be too viscous to handle. Typically a 0.1% or 0.2% solution is
prepared in two steps. First a 0.5% - 1.0% solution is prepared to allow for activation, then a
second dilution to 0.1 – 0.2% is made to allow for ease of handling and accurate delivery.
(i) Stock Solution Preparation. A 0.5% by weight solution contains 0.5g (or 500 mg) of
chemical in 99.5g (or 99ml) water, for a total of 100g. 1 ml contains 5mg of polymer.
a. Secure bottle cap and shake the polymer sample bottle vigorously for 1 minute before using.
2) Calculate the volume of liquid product to prepare 0.5% (5 g/L) active polymer stock solution.
Volume of polymer (ml) = (A x 100 x L)
S.G. x P
Where:
A = g/l polymer solution desired. (0.5% = (0.5/100) x 1000) = 5 g/l)
L = Total volume of solution being prepared. (250 ml = 0.250l)
S.G. = Polymer S.G. g/l supplied by manufacture.
P = Polymer % activity (MSDS or Product Data Sheet).

Example 1 : Stock Solution Preparation of Liquid Solution Polymer
Determine the volume of liquid solution polymer to prepare 250 ml stock solution containing 5.0
g/l (0.5%) of polymer by weight. Example has an S.G. of 1.022 g/ml and 7.25% activity.
Volume of polymer (ml) = (5.0 x 100 x 250/1000) = 16.87 ml.
1.022 x 7.25
Volume of water (ml) = 250 - 16.87 ml sample polymer = 233.13 ml.
Add 233.13 ml water and 6.87 ml of liquid polymer to a beaker and stir for approximately 5
minutes using a magnetic stirrer with stir bar.
Note: Use a disposable syringe to withdraw Liquid Solution Polymer from sample bottle.
Example 2 : Stock Solution Preparation of Liquid Polymer in Emulsion Form

Determine the volume of liquid emulsion polymer to prepare 250 ml stock solution containing 5.0
g/l (0.5%) of polymer by weight. The polymer has an S.G. of 1.068 g/ml and 38.0% activity.
Volume of liquid polymer in emulsion (ml) = (5.0 x 100 x 250/1000) = 3.08 ml
1.068 x 38.0
Procedure.
1. Add 246.02 ml water to a beaker. Adjust the stirrer rpm to give a large/strong vortex.
2. Add 3.08 ml emulsion polymer along the sides of the vortex and mix for approximately 10
minutes to ensure homogeneity. If a magnetic stirrer is not available, add water followed by
small but equal amounts of liquid polymer until the desired amount has been added.
3. Screw cap or lid on container and shake vigorously for 3-5 minutes.
Note: Use disposable syringe to withdraw Liquid Polymer in Emulsion from sample bottle.
(ii) Working Solution Preparation (2 g/L or 0.2%)

Procedure:
1. Make sure the sample bottle cap is secure and shake stock solution polymer sample bottle
vigorously for 1 minute in an up and down motion.
2. Place a beaker on top of magnetic stirrer and insert stir bar.
3. Determine the volumes required of stock solution and water, using the formula,
C2 = C1 x V1
V2
Where: C1 = Concentration of the initial polymer solution, (mg/l)
V1 = Volume on the of the initial polymer solution being diluted, (ml)
V2 = Total volume of the new solution, (ml)
C2 = Final Concentration of the new polymer solution, (mg/l)
Note: Multiply the % percent of the solution by 10,000 to convert to mg/L
For a 4 oz. 120 ml bottle, 2.0 = 5.0 x V1 / 120
Therefore V1 = (120 x 5)/2 = 48 ml.
4. Add 72.0 ml of water used at the rig location to the beaker. Turn on magnetic stirrer and
adjust the rpm to generate a large/strong vortex.

5. Using a clean syringe, withdraw 48.0 ml of stock solution from the appropriate bottle and
apply along the sides of the vortex. Purge the syringe 3 to 4 times.
6. Mix the working solution for approximately 5 minutes to make sure it is homogeneous.
7. Apply a small adhesive backed label to each bottle containing stock solution of each grade of
polymer prepared. Mark the name of the product, and solution strength.
8. It is recommended to discard working solution 24 hours from the time it was made.
9.10 PILOT TEST EXAMPLES

Example 1.
Measure 250 ml mud and add 250 ml of water for dilution. Stir well before adding coagulant.
500 ml of sample: Add 30 ml of 5% Polymer A coagulant solution to achieve pin flocculation
Add 12 ml of 0.5% Polymer B flocculant for large flocculation.
Dosages : Polymer A 30 x (5.0 X 10,000) = 3000 ppm
500
Polymer B 12 x (0.5 x 10,000) = 120 ppm
500
Determine lb/bbl of Dry Polymer from Pilot Test to Flocculate Mud

lb/bbl polymer = (PPM polymer / 1,000,000) x 350 lb/bbl
= (120 / 1,000,000) x 350 = 0.042 lbs/bbl
Determine Volume of Working Solution from Pilot Test to Flocculate Mud

To flocculate sample it takes 3,000 ppm Polymer A and 120 ppm of Polymer B. Both polymers
are 0.5% solutions.
If X = ml diluted polymer, polymer required = X/(% solution x 10,000) x ppm
Volume of Polymer A = 500/(5% x 10,000) x 3,000 = 30 ml
Volume of Polymer B = 500/(0.5% x 10,000) x 120 = 12 ml
Example 2.
How many lb/bbl of Polymer A are required to provide 600 ppm of polymer.
Convert ppm to % by weight to a fraction as follows (ppm = % by weight x 10,000),
600 = 100X x 10,000
100X = 600/10,000 = 0.06
X = 0.0006
Then convert fraction of % by weight to lb/bbl.
1 bbl of water weighs 350 lb/bbl ( 8.34 lb/gal x 42 gal/bbl = 350 lb/gal ).
Polymer dose to treat the fluid = 0.0006 x 350 lb/bbl = 0.21 lb/bbl
or lb/bbl polymer = ppm polymer / 1,000,000 x 350 lb/gal

9.11 Field Preparation of Polymer Solution Tanks with Solid Grade Polymers
9.11.1. Determine the number of usable gallons in the polymer solution mixing tank.
Length ft x Width ft x Height ft /5.62 bbl/ft3, (e.g. 5ft x 2ft x 3ft / 5.62 bbl/ft3 = 5.33 bbl)
9.11.2. Determine how many lbs of water is in the tank.

bbls x 350 lb/bbl = lb, (e.g. 5.33 bbls x 350 lb/bbl = 1,865 lb)
9.11.3. Determine how many lb of polymer to add to the tank to make a 1% by weight
solution.
ppm = % by weight x 10,000 (1% by weight = 10,000 ppm)
convert ppm to a fraction 10,000 = 100X x 10,000, X = 0.01
convert fraction to lb/bbl 0.01 x 350 lb/bbl = 3.5 lb/bbl
convert lb/bbl to lb 3.5 lb/bbl x 5.33 lb = 18.65 lb
9.11.4 Tank Preparation

The tank for mixing dry/solid polymers should be clean of all debris. A good agitation source,
such as that provided by a small lightning type mixer, which minimizes shear should be fitted to
the tank. Fill the tank with water to a level where the mixing blade is below the water level.
Measure the desired polymer required for the correct concentration with a scale. A typical
bathroom scale is accurate enough for our preparation. After weighing out the product add it to a
5 gallon bucket and mark the inside of the bucket with a marker. If other products are used it will
be necessary to re-mark the bucket as bulk densities change.
Utilize an eductor and fill the tank while educting the polymer into the tank. Once the polymer is
thoroughly mixed turn the mixer off to minimize shear degradation of the polymer. Hydrate the
polymer for a minimum of 30 minutes. Mix occasionally to maintain a homogeneous mixture.
If there is minimum agitation in the tank a liquid grade or rapid dispersion grade solid polymer
should be utilized. Rapid dispersion grade solid polymers are typically slightly more expensive
that typical solid grades due to coating the product, but they are not as expensive as liquid grades.
9.12 Field Preparation of Polymer Solution Tanks with Liquid Polymers

Liquid grade polymers are more expensive that solid grade polymers because of the emulsion or
dispersion process. Emulsions have 3 phases, water, oil, and polymer. Dispersions have 3
phases, less water than emulsions, oil, and polymer. These liquid products have numerous
surfactants and different types of carrier oils.
Liquid grade polymers should only be used where proper mixing is a problem, as the treating cost
per unit volume of fluid will increase significantly. Also the oils and surfactants may need to be
evaluated if the effluent is being discharged into the environment. Typically the manufacturer
will give the activity of the emulsion or dispersion. The % active solids must be known to
prepare the solution polymer needed to properly flocculate the fluid.

Example:
Polymer A is 50% active with a density of 8.8 lb/gal
Concentration = 0.50 x 8.8 lb/gal = 4.4 lb/gal (1 gallon of liquid polymer has 4.4 lb of polymer)
If 18.65 lb of polymer is required to make up a 1% solution, how many gallons of polymer should
be mixed in the tank?
18.65 lb/ 4.4 lb/gal = 4.2 gals Polymer A
9.13 Application Rate of Polymer Solution

Once the dose rate has been determined and the solution tanks made up, the polymer solution
injection pump must be set at the proper rate to give the determined ppm from the pilot test.
1. Determine lb/bbl of polymer to treat fluid from the pilot test. In the previous example it was
determined to be 0.21 lb/bbl to treat for a 6600 ppm application.
2. Determine the polymer solution concentration in lb/bbl or lb/gal. In the example a 1% or 3.5
lb/bbl solution was mixed. The tank volume was calculated as 5.33 bbl and 18.65 lb of total
polymer was required to make up a 1% solution.
3. Determine feed rate of the drilling fluid that will be feed to the centrifuge. This can be done
with a simple flow meter or by physically checking by measuring a given volume. Assume that
the rate is 100 gal/min of drilling fluid.
4. How many bbl drilling fluid can be treated with a 1% solution for a treatment of 600ppm.
18.65 lb / 0.21 lb/bbl = 88.8 bbls
5. If the feed rate to the centrifuge is 100 gal/min how many gal/min of 1% polymer solution
should be injected?
a. Convert treatment concentration from lb/bbl to lb/gal.
lb/bbl / 42gal/bbl = lb/gal
0.21 lb/bbl /42 gal/bbl = .005 lb/gal
b. Determine lb/min of polymer.
lb/gal x gal/min = lb/min
0.005 lb/gal x 100 gal/min = 0.5 lb/min
c. Convert polymer solution from lb/bbl to lb/gal

lb/bbl / 42 gal/bbl = lb/gal
3.5 lb/bbl / 42 gal/bbl = .0833 lb/gal
d. Determine rate of polymer solution.
treatment conc. lb/min / sol conc. lb/gal = gal/min
0.5 lb/min / .0833 lb/gal = 6 gal/min
Inject 6 gal/min of a 1% polymer solution for a feed rate of 100 gal/min to the centrifuge for a
600 ppm treatment.

9.14 Guide for Dewatering Spreadsheet
This Spreadsheet is intended as a guide to mix polymer solution for pilot testing, which will give
mixtures for hydrating polymer in blending tanks and estimated de-watering cost if all variables
are included. Gray area is for data entrees of each polymer.
1. Put down the estimated barrels of fluid to treat.

2. Enter percentage polymer strength desired. Suggest- Coagulants range 5%-0.5% &
Flocculent range 1.0 % to 0.05%
3. Desired amount of working solution for pilot testing. Suggest 500 ml or less depending on
strength and amount of testing.
4. Specific gravity of liquid polymer. See MSDS or Product Data sheets.
5. (%) Percent activity or weight of polymer. See MSDS or Product DATA Sheet.
6. Enter desired barrels of working solution to build.
7. Enter percent polymer strength desired. Suggest range on Coagulants from 5% to .5%.
8. Desired amount of working solution for pilot testing. Suggest 500 mL or less depending on
9. Enter percent polymer strength desired. Suggest range on Flocculent from 2% to .1% due to
thickness from structure of long chain Polyacrylamide type polymers.
10. Desired amount of working solution for pilot testing. Suggest 500 mL or less depending on
Information from pilot test results:
11. Amount of mud or stock fluid used for pilot test. Suggest 100 ml to 500 ml.
12. Amount of dilution (Water) in ml added to mud or stock fluid.
13. Amount of liquid Coagulant-working solution added to stock fluid or mud in pilot test
measured in ml.
14. Amount of powdered Coagulant-working solution added to stock fluid or mud in pilot test
measured in ml.
15. Amount of powdered Flocculent-working solution added to stock fluid or mud in pilot test
measured in ml.
16. Estimated feed rate into centrifuge measured in GPM.
17. Enter the cost per pound of liquid coagulant polymer in the shaded gray area.
18. Enter the cost per pound of powdered coagulant polymer in the shaded gray area.
19. Enter the cost per pound of liquid flocculent polymer in the shaded gray area.
20. This space for acid or any other type chemical added to mud or stock fluid before processing.
Enter pounds per barrel in light blue area and cost of 50-pound sack in gray area.
21. If water or dilution fluid has a cost, enter data in gray area.
22. This space for Bentonite or any other type chemical added to mud or stock fluid before
processing. Enter pounds per barrel added in light blue area and cost of 100-pound sack in
gray area.

MIXTURE FOR LIQUID AND POWDER POLYMERS
(1) Total Barrels De-Watered 200 bbls
Liquid Solution Polymers
Name of Polymer Mixing
(2) Percent mixture desired (5% to .5 % ) 1.5 %
(3) Milliliters of Working Solution 500 mL
(4) Specifies Gravity of Polymer or measured in g/mL 1.3 S.G.
(5) % Percent Activity of Polymer (Product DATA Sheet) 32.5 % by Wt.
(6) Amount of Liquid Solution Volume to mix in Pit 40.00 bbl's
Volume of Liquid Polymer to Mix 17.75 mL
Volume of Water to Mix 482.25 mL
Volume of Liquid Polymer to Mix 59.645 gallons
Volume of Water to Mix per 38.580 barrels
Powder Solution Coagulant Polymer
(7) Percent mixture desired (.5% to .1 % ) 3%
Polymer Type and Name:
Weight of Powder Polymer to Mix 15.79 Grams
Weight of Powder Polymer to Mix in pit 31.5789 kg/m3
Weight of Powder Polymer to Mix in pit 11.05 lbs/bbl
Powder Solution of Flocculent Polymer
(9) Percent mixture desired (.5% or .1 % ) 0.25 %
Polymer Type and Name:
Weight of Powder Polymer to Mix 1.32 Grams
Weight of Powder Polymer to Mix in pit 2.6316 kg/m3
Weight of Powder Polymer to Mix in pit 0.92 lbs/bbl
Injection Rates Based on Laboratory Test
(11) mL of Coagulant added to Stock Mud 30 mL
(12) mL of Flocculent added to Stock Mud 12 mL
(13) Amount of Stock Mud or Fluid 250 mL
(14) Dilution added (Water) 50 mL
(15) Feed rate of mud into centrifuge 25 gpm
11.36 Lt/Min
Injection Rate of Liquid Coagulant 3 gpm
11.36 Lt/Min
Injection Rate of Powdered Coagulant 3 gpm
4.54 Lt/Min
Injection Rate of Powdered Flocculent 1.2 gpm
18.93 Lt/Min
Injection Rate of water for dilution 5 gpm
Cost per Barrel of Fluid De-Watered
(16) Coagulant Cost (Liquid Concentrate) 0.38 cost/lbs $0.74 cost/bbl
(17) Coagulant Cost (Powder ) cost/lbs 0.00 cost/bbl
(18) Flocculent Cost 0.25 cost/lbs 0.09 cost/bbl
(19) Acid Cost (Citric Acid lbs) 3 75 cost/sack $1.13 cost/bbl
(20) Water Cost cost/bbl cost/bbl
(21) Miscellaneous (Bentonite lbs 2 6.02 cost/sack $0.06 cost/bbl
Cost per Barrel of Chemical to De-Water Fluid $2.01 cost/bbl

9.15 Laboratory Procedures for Oil-Based or Synthetic Drilling Fluids
9.15.1 Required Equipment
For laboratory testing the following equipment is required:

(i) Laboratory centrifuge able to hold 50ml centrifuge tubes and generate at least 750G’s.
e.g. International centrifuge, model SBV, Size 1, fixed angle, or MSE Mistral 2000. Other
centrifuges may be used provided they can generate a similar G force.
(ii) Disposable plastic centrifuge tubes, 50ml.
(iii) High shear overhead mixer (e.g. Silverson, Premier Mill)
(iv) 250ml plastic beakers or disposable plastic cups.
(v) Mixing spatulas
(vi) Disposable syringes, 2ml, 5ml, 10ml.
(vii) Samples of EMR 707, various surfactants, base oil and water.
9.15.2 . Laboratory Procedure

The following procedure covers the method for the evaluation of polymer-based flocculants in
combination with demulsifying surfactants in removing fine solids from OBM/SBM.
(i) Mix the mud sample using an overhead mixer until the sample is homogeneous. Retrieve a
sub sample after mixing and carry out a full mud check to determine the mud properties.
(ii) Weigh out a 50ml mud sample into a 250ml plastic beaker.
(iii) Using a disposable syringe, inject polymer into the mud sample, around 2 – 5% volume is a
good starting point. Stir the polymer in using a spatula until the composition is
homogeneous.
(iv) Observe the physical state of the treated muds and comment. The use of qualitative terms
such as “fluid mud”, “soft pudding”, grainy mud”, “elastic mud” or any combination of
these phrases is suggested. Figure 9.5 below shows an example of flocculated mud with a
“soft pudding” appearance.
Figure 9.5 - Flocculated Mud Figure 9.6 - 50ml centrifuge tubes after spinning
for ten minutes at a centrifugal force of 720 G’s.
(v) Generate a dose response curve by adding 1- 6% by vol. polymer to the mud samples.
(vi) Add the treated muds to 50ml centrifuge tubes and spin for ten minutes at 720 G’s.
(vii) Observe the physical state of the centrifuged mud. Note the volume of each layer, and its
general physical character, e.g. compacted solids, slurry, water, emulsion and oil.
Also note the amount of solids retained in the upper liquid phase and assign a suitable
description e.g. “very dirty oil”, “dirty oil”, “slightly dirty oil”, “clean oil” etc. A good way

to assess this is to dip a clean spatula into the upper liquid phase, invert it and observe how
the fluid drains down the spatula. A good estimate of the solids loading in the oil can thereby
be made as is shown in Figure 9.6.
Figure 9.7. Oil phase from centrifuged mud with no polymer,
2%v polymer treatment and 4%v polymer treatment
(viii) After treating with polymer alone, the following testing matrix should be followed. It
incorporates the use of base oil, water and a selection of surfactants which may improve
separation.
(ix) Dilute the polymer in the base oil of the mud being tested (1:1 v/v), add to the mud, mix
until composition is homogeneous and repeat stages 4 to 7. Test in the range of 2 – 4% by
vol. polymer to determine the optimum dosage. A stock solution of dilute polymer may be
made up but should be made fresh every day.
(x) If little or no separation is observed try adding surfactants. Choose a surfactant and add at
around 2 - 4%vol. Mix until homogeneous then add diluted polymer and repeat stages 4 to 7.
(xi) If little or no separation is observed, add water (tap water is sufficient) at around 10% vol.
and mix until composition is homogeneous. Then add and mix in the surfactant followed by
the diluted polymer and repeat stages 4 to 7.
Note: Good procedure also involves taking photographs of the centrifuged mud for future
reference. Photographs of the flocculated mud before and after centrifugation are advisable. It
may also be useful to photograph how the top phase drains down a clean spatula, as shown above
in Figure 3, in order to record some information on the solids loading of the upper phase.

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Section 9 : Dewatering Procedures

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9.1 Selecting the Most Efficient Dewatering Additives

9.1.1 Summary of the Dewatering process

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Table 9. 2 Optimum pH Range for Inorganic Coagulants

Table 9. 3 Advantages and Disadvantages of Inorganic Coagulants

Dewatering Manual v 1.0 135

Dewatering Manual v 1.0 136

Figure 9.1. Polymers and Flocculation Applications

Dewatering Drilling Mud Paper effluents

Dewatering Secondary Sludge

Dewatering Alkaline Sludge

Sugar applications Raw Water Clarification and

100% 50% 0% 50% 100%

Adapted from D.A. Mortimer (1991) Polymer Int. 25, 29-41

9.1.4 Factors Effecting Coagulation and Flocculation

Dewatering Manual v 1.0 137

Influencing Factor Coagulation Flocculation

9.2 Pilot Testing Procedures

9.3 The Jar Test

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Figure 9.3. Jar test Apparatus

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9.5 Testing in the Laboratory.

9.5.2 Dilute the Test Fluid

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9.5.3 Choice of Working Solution Concentrations

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9.5.5 Determine the Optimum Flocculant Polymer Dose.

Dewatering Manual v 1.0 142

Table 9.8 : Example Testing Program for Flocculant Dose.

9.5.6 Fine Tuning the Optimum Doses and Dilution Requirement.

9.6 Field Testing

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9.8 Standard Field Test Procedures

9.8.2 Step 2 : Choice of Working Solution Concentrations

9.8.2 Step 3: Determine if pH Adjustment Needed

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9.8.3 Step 4: pH Adjustment

9.8.4 Step 5: Flocculation of pH Adjusted Drilling Fluid Sample

9.8.5 Step 6: Flocculation of Drilling Fluid Which Requires Coagulation

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9.9.1 Recommended Pilot Testing Equipment required:

9.9.2 Preparation of Inorganic Coagulants.

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9.9.3 Preparation of Powder or Granular Polymer

Preparing a 0.5% stock solution

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Preparing a stock solution

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Example 2 : Stock Solution Preparation of Liquid Polymer in Emulsion Form

(ii) Working Solution Preparation (2 g/L or 0.2%)

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9.10 PILOT TEST EXAMPLES

Determine lb/bbl of Dry Polymer from Pilot Test to Flocculate Mud

Determine Volume of Working Solution from Pilot Test to Flocculate Mud

Dewatering Manual v 1.0 151

9.11.2. Determine how many lbs of water is in the tank.

9.11.4 Tank Preparation