Demilusfier bottle test

The Bottle Test is performed to assist in the selection of the treating compound that will most
effectively break the emulsions from any given well, lease, or field. The Bottle Test results may
also be used as an indication of the ratio of treating compound to emulsion, which will be
required to achieve salable oil.

There are some basic rules that need to be followed in carrying out a proper and informative
Bottle Test.
• The sample used for the Bottle Test must be chemical free and representative of the
emulsion to be treated. If possible, always use a composite sample.
• The sample should be as fresh as possible because rapid aging of some emulsions affects
their susceptibility to treating.
• The same conditions of agitation, heat, dosage, and retention time as are found on the
lease should be simulated as closely as possible. The system survey should also note any
recent changes in the field, chemicals, workovers, etc.

The Bottle Test is performed in three separate functions: Ratio Test, Elimination Test, and
Confirmation Test. These are described briefly below.

Ratio Test
The Ratio Test is the first function of the Bottle Test. Normally, the compound in use for the
emulsion is dosed at different levels to determine the proper dosage for treatment. A general rule
of thumb is to dose the compound at three levels below and three levels above the existing rate.
The Ratio Test prevents wasting time in the Elimination Test by dosing too low (resulting in no
treatment) or dosing too high (resulting in too many compounds giving good results and possibly
resulting in overtreatment). The Ratio Test is also where the parameters of the Bottle Test are
defined. This is where, based on system information, agitation, dosage, heat, and retention time
are determined to produce salable oil with the compound in use.
An overtreat ratio (three to five times the normal treating rate) indicates if overtreating is a
problem. If at all possible, avoid products that overtreat. The low ratio, below the treating rate,
exaggerates treating differences and helps select the best product.
Elimination Test
The second function of the Bottle Test is the Elimination Test. After the test parameters have
been determined, the bulk of the testing will be accomplished during the Elimination Test.
Instead of dosing one compound at several ratios, many compounds will be dosed at the same
ratio. Sometimes, many compounds are dosed at several ratios. The ratio to use will be based on
the results of the Ratio Test. The Elimination Test is completed when all the desired compounds
have been screened and several promising ones have been identified.
Re-emulsification Test
After grindouts have been obtained, re-mix the separated emulsions of the best chemical
candidates to determine which do not re-emulsify.

Confirmation Test
The Confirmation Test is the last function of the Bottle Test. The Confirmation Test is nothing
more than a Ratio Test with the best compounds identified during the Elimination Test. Several
ratios below and several ratios above the dosage that gives salable oil should be run. The results
of the Confirmation Test should:

• Determine the best compound that treats this emulsion to pipeline oil.
• Indicate the optimum and range of the dosage.

Bottle Test Results

During the Bottle Test, compounds are evaluated and observations are made on several criteria.
These observations are recorded on a Bottle Test Report form for comparison study and as a
permanent record of knowledge. Below are the main criteria recorded on the Bottle Test Report
for the evaluation of emulsion breakers.

1. Water Drop
Water drop is defined to be the water that coalesces and settles to the bottom of the
prescription bottle. The relative speed of the breaking of an emulsion is usually indicated by
the speed of water drop. The speed of water drop can be misleading. Sometimes a compound
will show rapid initial water drop and then stop before all the water is released. The best
water drop is both fast and complete. The importance of the speed of water drop depends on
the system treating the emulsion. Generally, as the retention time is increased, the importance
of speed is decreased. It is generally advisable not to select a product that drops water much
faster than the system residence time.

2. BS&W Content of Oil

BS&W stands for basic sediment and water. Basic sediment is usually unresolved emulsion
but can also include organic and inorganic solids. BS&W can be distinguished in crude oil by
a trained and experienced Bottle Tester using the naked eye. As the BS&W content
decreases, the deeper the color and brighter, or polished looking, the oil layer becomes. The
best and most accurate way to measure BS&W content is to perform a thief grindout and slug
grindout on the oil. The thief grindout measurement tells how well the emulsion is resolving
and how complete is the water release or dehydration. The slug grindout tells if there is any
secondary emulsion in the oil. Secondary emulsion is a new term that will be defined and
distinguished from normal, or primary emulsion, as follows:

a. Primary Emulsion
The BS that is thrown down on centrifuging a sample of crude oil without the addition of
an excess (slug) amount of treating chemical. Primary emulsion is thrown down as a
more or less well defined layer.
b. Secondary Emulsion
The additional amount of BS which is present in the grindout tube which did not pack
down on centrifuging and which on treatment with an excess (slug) of chemical is broken
down to oil and water. The presence of secondary emulsion results in the water reading of
the slug grindout to be larger than the sum of the BS and water readings of the unslugged
grindout.
Generally, the best compound will be the one that has the lowest slug grindout with the least
amount of BS in the unslugged grindout.
If there is a question whether the sediment is paraffin or emulsion, the centrifuge tube may be
heated. If the sediment separates with heating to show water and oil, it is emulsion. If the
sediment melts and no water appears, tilt the tube. Paraffin will resolidify along the side of
the tube.

3. Interface
In the ideal treatment of crude oil emulsions, the oil-water interface should be a sharp, clean
line without any web or sludge. Presence of a considerable amount of sludge or web is
undesirable. In a treating plant, this foreign material will eventually go to stock and be
reported as BS. Trace amounts of web or sludge seen in the Bottle Test, however, may
disappear or treat out in the treating plant. Foreign materials at the interface can often be seen
through visual observations and are recorded for reference. Sometimes, the condition of the
interface is not easily seen and needs a more accurate method of evaluation. The composite
grindout is the tool used to determine the quality of the oil contained between the oil-water
line and the level at which the thief grindout was taken. Some compounds are referred to as
“sludgers.” This means that they give good thief grindouts but make sludge of water, BS, or
both at the interface. These compounds may yield clean oil for a time, but eventually a pad
will build and grow at the interface, spilling over to stock and causing bad oil. The composite
grindout will reveal this potential problem.
4. Water Quality
During Bottle Tests, water quality is noted and recorded for reference. Concern for the
environment, injection well plugging, formation damage, and increased treating cost are a
few reasons why water quality is important in treating regular emulsions. Although most
production facilities have water treatment systems, it is important not to add to or create
water problems with regular emulsion breakers. Selecting an emulsion breaker compound
that produces clean oil and clean water is the ultimate goal.
High RSN demulsifiers or wetting agents (surfactants) can cause cloudy water by dispersing
oil in the water phase, especially in freshwater. In high TDS water, higher RSN products may
be used without oil-in-water problems.

5. Treating Range
Compounds with the widest treating range that yields good emulsion treatment are preferred,
but not always the best for a certain application. Wide treating range products are better able
to handle fluctuations in product rates, system upsets, and temperature changes and are easier
to introduce into a treating plant. Wide treating range compounds also help overcome the
tendency of field operators to increase dosages when system upsets occur. If this happens and
the compound goes into an overtreat condition, this attempted solution can make the problem
worse than the original problem.
Testing on a composite sample over several days is recommended to insure consistent
demulsification. If you select an emulsion breaker based on samples from one well, there is a
chance the product may not be effective for the entire field.
The treating system may dictate the importance of one factor to be weighted more heavily than
another; but all of these criteria should be considered when evaluating emulsion breakers by the
Bottle Test. The Bottle Test is not an exact science, only a tool to aid in the selection of
emulsion breaker compounds. It is a static test performed on a dynamic system and cannot
duplicate the true fluids. Nevertheless, the Bottle Test remains the industry standard for
emulsion breaker evaluation.
The Bottle Test

The following describes the steps in the Bottle Test in detail.

Field System Survey

first step is the most important step in doing a regular emulsion breaker Bottle Test right the
first time. By going through this procedure, your emulsion breaker Bottle Testing will produce
more accurate and meaningful results. Deleting the Field System Survey from your Bottle Test
procedure may cause you to make inaccurate or insufficient interpretations of the test results. In a
worst case, failure to perform a good survey might ruin your chances at a successful proposal or
plant test.

Ratio Test
1. Complete all known information on the Bottle Test Report. If you should have a problem
interpreting your Bottle Test results, other OFC personnel can assist you.
2. Obtain a chemical-free sample of crude oil emulsion.
3. Drain all free water from the sample. Add free water back to each bottle to give a water/oil
ratio that reflects the production. Never exceed a total water amount in the bottle of 60%.
This free water will closely mirror results of the emulsion breaker treatment in the initial
separation and indicate potential water quality problems.
4. Shake the sample container to obtain a homogeneous sample for a grindout.

Centrifuge two samples: one chemical free, the other slugged with a few drops of cut
EC2003A. Straight EC2003A is not normally used, as an overtreat can sometimes occur.
EC2003A is usually cut back with a solvent (R-3533, R-3320, etc.) to 50:50, 30:70, etc.,
depending on your experience and area. DO NOT USE GASOLINE as a solvent in any
emulsion breaker test. Gasoline contains emulsion breakers!

5. Fill seven bottles to the 100 ml mark with freshly collected crude oil emulsion and invert
several times, so that the bottles will be coated with an emulsion film. The seventh bottle will
be the blank.
6. Make a 10% solution of the formula being used in the system only when the API° gravity of
the oil is less than 18° gravity, otherwise use the drum strength solution, and pipette chemical
concentrations: three below and three above the existing rate. Example: if the chemical
concentration in the system is presently 120 ppm, the concentrations of 50, 80, 110, 150, 180
and 200 ppm plus the blank could be evaluated.
Note: Any 10% emulsion breakers should be made with a Nalco Energy Services solvent
such as R-3533, R-3320, etc. DO NOT USE GASOLINE.
7. Cold agitate bottles to ensure adequate dispersion of chemical in the emulsified oil.
• The amount of agitation is determined from the field system survey and the amount of
agitation occurring in the system between the point of demulsifier injection and the
treating vessels.
• Cold agitation means at the temperature of the fluid taken at the demulsifier injection
point or at the inlet to the treating vessels. Example: if the fluid temperature at the
injection point is 60°F, then agitate at 60°F; if the temperature at the injection point is
140°F, cold agitation should be at 140°F.

8. If the emulsion requires heat for treatment, place the bottles in a water bath adjusted to the
treating vessel temperature.
9. Every few minutes examine the bottles carefully and record water drop, the presence of a BS
layer, and general appearance on the Bottle Test Report.
A rule of thumb for the time period between readings: only take readings if there has been a
significant change in water drop in one or more bottles since the previous reading.
10. After some time, based on many bottles showing good water drop and the information
gathered from the Field System Survey, agitate a second time (hot agitation). Cold treating
may also see a second agitation, depending upon your Field System Survey.
11. After hot agitation, record water drop, presence of a BS layer, and general appearance on
the Bottle Test sheet.
12. After maximum water drop is achieved, based on the grindout from Step 11 above, perform
the Thiefing Grindouts on the treated crude oil samples:
a. Fill a centrifuge tube to the 50% mark with some type of suitable hydrocarbon solvent
(Stoddard Solvent, White Gas, Toluene, R-3533, etc.). DO NOT USE GASOLINE.
b. Select the bottle with the most water drop volume. Adjust a thief pipette so that an oil
sample can be taken from a point 15 ml above the water level in this bottle. Use this
setting for thiefing all the bottles in this test. Do not adjust the thief level for each
bottle.
c. Draw oil from the first bottle and fill the centrifuge tube to the 100% mark. Mix the oil
and solvent in the tube by shaking. If paraffin is present, heat the tubes if necessary to
d. Continue this process with all of the treated samples.
e. Record the water and remaining BS in their proper columns on the Bottle Test Report in
the section labeled “Thief Grind Out.”
13. Run an excess chemical grindout on each centrifuge tube:
a. Add two to three drops of cut EC2003A to each centrifuge tube and agitate each tube
vigorously, making certain than any BS layer is broken up.
b. Heat the tubes if paraffin is present.
c. Centrifuge three to five minutes and record the results in the section of the Bottle Test
Report labeled “Slug” (“Excess” on some forms).
d. Record any presence of unbroken BS, the color of water at the bottom of the tube, and
any solids at the bottom of the tube.
14. Some systems require a Composite Grind Out for meaningful data. Field experience will
tell you if this needs to be done. This procedure requires you to:
a. Extract, with a pipette, all the free water at the bottom of each bottle.
b. Fill centrifuge tubes to the 50% mark with a proper hydrocarbon solvent.
c. Recap each bottle and shake vigorously to make the remaining oil-water emulsion
homogenous.
d. Immediately pour a sample from each bottle into the centrifuge tubes, filling to the 100%
mark.
e. Centrifuge, as in the Thief Grind Out, and record results for water and BS in the section
of the Bottle Test Report labeled “Composite Grind Out.”
f. Perform an excess chemical grindout with cut EC2003A, as in the Thief Grind Out and
record.
Elimination Test Procedure
1. Select the OFC formulas that your past experience indicates to be of value for the type of
emulsified crude in question.
a. Take this opportunity to test all new OFC compounds for your records.
b. Always include the emulsion breaker used in the field you are testing, whether it is an
OFC product or one of the competitor’s. The emulsion breaker Bottle Test is not valid
without it!
2. Follow the same procedure as in the Ratio Test except that now you will inject several
products at one ratio rather than one product at several ratios. The ratio to be used will be
based on your observations in the Ratio Test. In the Elimination Test, you want to find a
product that performs better than the one currently in the system; therefore, the Elimination
Test should be run at a ratio that did not quite produce pipeline oil in the Ratio Test.
Example: in the Ratio Test the product currently in the system was treated at 60, 90, 120,
150, 180, and 210 ppm. Pipeline oil in the system is <1.0% BS&W. Thief grind out were less
than 1.0% at the ratios 150, 180, and 210 ppm. The Elimination Test should be run at a ratio
less than 150 ppm, perhaps at 120 ppm.
3. It is strongly recommended that two or three ratios of each product be tested, rather than
just one, if time permits. A two or three Ratio Test of each product will give meaningful
information regarding treating range.
4. From the above procedures, the best three or more OFC emulsion breakers plus the emulsion
breaker currently being used in the field should be chosen for further evaluation in the
Confirmation Test.

Confirmation Test Procedure

1. The Confirmation Test is run exactly like the Ratio and Elimination Tests, except that only
the OFC products that performed the best in the Elimination Test are used.
a. The test is run at two ratios below and one ratio above the ratios used in the Elimination
Test.
b. The purpose of this test is to remove all doubts as to which OFC emulsion breaker is right
for the emulsified crude in question.
c. Again, this test must also include the emulsion breaker currently used in the field.

2. After the Ratio Test, Elimination Test, and Confirmation Test have been completed, the OFC
product best for the system is determined by considering these factors:
a. Relative speed of the breaking of the emulsion, which is usually indicated by the speed of
water drop.
b. The color and brilliance of the oil layer.
c. The color and brilliance of emulsion/oil remaining on the top section of the bottle.
d. The appearance of the oil-water interface. The best performance is usually indicated by a
clean, smooth break and the absence of any so-called “webby” or “raggy” material.
e. The ability to most nearly produce treated oil to pipeline specifications. This means the
lowest BS&W results both before and after slugging with EC2003A.
f. The product that drops the cleanest water. Cloudy, dirty water produced by an emulsion
breaker in the Bottle Test may indicate that the product would cause overboard or water
injection problems.
Bottle Testing Systems Making Less than 50 bbls Oil per Day (BOPD)
1. When Bottle Testing Systems making less than 50 BOPD, the ratios used in the Bottle
Testing must be adjusted to account for the fact that most chemical injection pumps will not
pump at a rate less than one quart per day.
2. First, determine the amount of oil and water produced.
3. Assume that the chemical pump can pump a minimum of 1 quart per day effectively.
4. Calculate the ratios to use in each test based on the use of 1 quart per day of product.
Example: the lease makes 15 BOPD and 15 BWPD. In your Ratio Test, you would use the
equivalent of one quart of chemical per 15 barrels of oil, one quart of chemical per 20 barrels
of oil, one quart per 25 barrels of oil, etc.; or about 400 ppm, 300 ppm, and 240 ppm
respectively. These ratios are calculated using the formula:
Ratio, ppm = 5,925 / bbl oil
5. This adjustment allows you to simulate the system and conduct your testing under more
realistic conditions. The emulsion breakers used under these conditions usually are either less
active or have a wide treating range.
Interpretation of Results
1. Speed of Water Drop
The speed of water drop can be misleading, because occasionally an emulsion breaker will
show rapid initial water drop and then stop before all the water is released. Consider only
those emulsion breakers that release all of the water.
2. Color and Brilliance of Oil
The color and brilliance of oil in transmitting light is very important and a trained observer
can detect the presence of BS&W with the naked eye. Generally, the brilliance and the depth
of color increases with the decrease in BS&W content.
3. Oil-Water Interface
In the ideal treatment of crude oil emulsions, the oil-water interface is sharp and clean
without any web, rag, or sludge present.
4. Water Quality
The water at the end of the test should be crystal clear. Cloudy, dirty water produced by an
emulsion breaker in the Bottle Test may indicate that the product would cause quality or oil
carry-over problems in the system.
5. Low BS&W
The lowest BS&W readings in the grindouts, along with the water quality and rapidity of
water drop in the allocated treating time, will indicate which of the treating emulsion
breakers evaluated would be the initial choice to be plant tested.
6. Additional Factors
a. Dispersibility of OFC emulsion breaker in the produced waters.
b. Success of selected OFC emulsion breaker at other locations in your area.
c. Availability of selected OFC emulsion breaker.
d. Cost-effectiveness of selected OFC emulsion breaker.
e. Your experience in the area with the type of emulsified crude you are testing.