Bony Budiman

DEMULSIFIER BOTTLE
TEST
BONY BUDIMAN
2021
 Bony Budiman

COMMON QUESTION

• What is demulsier botte test ?

• How to conduct the bottle test ?
• What shall be considered ?
• Examples how to design bottle
test

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OUTLINE

• OBJECTIVE
• INTRODUCTION
• BOTTLE TEST DESIGN
• FORMULATION
• STABILITY TEST
• EXAMPLES
• SUMMARY
 Bony Budiman

OBJECTIVE

Oil • Know basic principle of

Oil Oil
demulsifier bottle test

Oil Water • Prepare bottle test design

Oil by considering the specific
target and field condition
Oil
Oil
Oil
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INTRODUCTION

• The aim of demulsifier bottle test is to

break the water in oil emulsion
• Parameters that analyzed during
demulsifier bottle test :
• Water cut (BS&W)
• Water drop
• Interface
• Water clarity
• Salt content
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WATER CUT (1)

• Technically known as Basic Sediment and

Water (BS&W)
• Water cut is parameter to check remaining
water and emulsion in the crude oil.
• General procedure :
• Thieve the crude oil using syringe to the
centrifuge tube
T,t
• Centrifuge refer to ASTM No D4007
BS&W by Centrifuge
• Read the amount of sediment (solid), water
and emulsion
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WATER CUT (2)

• This is an example how to read the BS&W

• Oil interface is below value 0.5 %, means each scale strip equal to 0.05%
• Refer to ASTM D4002, we add 50% toluene to 50% sample so the result
shall be multiply by 2
• Total BS&W has 8 strips  BS&W = 8 * 0.05% * 2 = 0.8 %
• Emulsion has 1 strip,  1 * 0.05% * 2 = 0.1%
• Water has 4 strips  % Water = 4 * 0.05% * 2 = 0.4 %
• Sediment = Total BS&W – emulsion – water = 0.8 – 0.1 – 0.4 = 0.3 %
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WATER CUT (3)

• There are 4 type of water cut : top cut, middle cut, bottom
cut and mix cut
• Top cut : sample taken in the 20% up of the oil layer.
Important parameter if use the spill over separator
• Middle cut : sample thief around 50% of oil layer.
TOP
CUT • Bottom cut : sample thief 20% below of the oil layer
MIDDLE • Mix cut : sample thief from top, middle and bottom.
CUT
Important parameter if use full settling separator
BOTTOM
CUT
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WATER DROP

• Water drop is how much water separated from the crude

oil.
• More water separate means better emulsification process
• There are some kinds of water drop : fast water drop and
total water drop
• Fast water drop : if the water immediately separate in
minutes after demulsfiier treatment
• Total water drop : total water separation after specified
settling time
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INTERFACE

C D • Interface is parameter that show how good the

A B
boundary between oil and water phase.
• Good demulsifier will provide sharp/clear/thin
of interface
• Thick interface will interfere the separator level
and calculate it as hydrocarbon phase.
• In picture beside, the A bottle provide best
interface and the D bottle is the worst.
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WATER QUALITY

• The separated water should not contain as less as

possible of oil. This parameter is shown visually by
the water clarity.
4
1 2 3 • Some demulsfier has performance to provide good
water clarity.
• At picture beside, demulsifier 4 has best water clarity
performance while demulsifier 1 is the worst
• This parameter important for some reasons :
• Reduce further water treatment process
• Increase oil export volume

Courtesy picture : https://pubs.acs.org/doi/pdf/10.1021/ef101087u?rand=cwpl0v4a

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SALT CONTENT

• Salt in crude not expected in the crude oil

since it will cause corrosion especially at
refinery process plant.
• Salt usually dissolved in water. Separate water
as much as possible usually decrease salt as
well. However some salts may trapped in the
crude oil.
• Specification of salt in crude vary from 5 to
maximum 20 pound per thousand barrel (PTB)

Courtesy picture : https://www.stanhope-seta.co.uk/product/salt-crude-analyser/

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BOTTLE TEST FLOW

DESIGN SAMPLING LABORATORY
TEST

• System • Equipment • Reagent and

Review • Sampling Equipment
• KPI Point • Ratio Test
• Procedure • Quality • Intermediate
• Quantity Screening
• Synergy
• Formulation
• Optimization
• Stability
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DESIGN : SYSTEM REVIEW

• Check all wells especially wells with :

• High production
• Tight emulsion
• The hottest and the coldest

• Check the separation process :

• Type of separator
• Temperature
• Retention time

• Demulsfier injection point

• Others chemicals injection especially
Corrosion Inhibitor
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DESIGN : KPI (1)

• From the design review, we shall determine the Key

Performance Indicator (KPI)
No Parameter Specification
• Each demulsfier may not works to make good oil, fast-
1 Top cut oil < 0.6% maximum water drop, clear water, sharp interface and
2 Total water drop 60 % in 4 hours low salt content.
3 Water quality Clear water • Our target in bottle test demulsifier is to find
4 Salt content Max 7 ptb demulsfier that could work to support sales
specification by considering the field process
condition.
• Demulsifier with top oil charectiristic will be enough
for spill over washtank type, even the interface is jaggy.
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DESIGN : KPI (2)

• During bottle test, the result shall be

written in the observation table form
• The form consist of parameters that
determined as KPI
• Each bottle tester has a special form
and a different way of filling out the
table from each other.

Courtesy picture : https://patents.google.com/patent/WO2009094221A1/en

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DESIGN : PROCEDURE

• The procedure is guideline to ensure that the bottle test

mimic the field condition and considering the KPI
• The procedure may specific for each field
• The procedure of demulsifier bottle test may consist of :
• Reagent, instrument, tools and supporting kit
• Liquid composition
• Shaking type
• Settling time
• Demulsifier formulation
• Thief position

Courtesy picture : http://toeflstrategy.blogspot.com/2016/04/contoh-procedure-text-lengkap.html

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SAMPLING : EQUIPMENT

N Equipment Function Remark

o
1 Hose and To flow sample from the Some sampling point require
Connection sampling point to sample reducer or enlarger connection
container
2 Sample To store sample Metal with grounding is preferred
container
3 PPE To ensure safety during Safety helmet, shoes, wearpack,
sampling googles ,gloves and gas detector.
4 Wrenches To open sampling point
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SAMPLING : SAMPLING POINT (1)

• It is important to get
representative sample from the
sampling point.
• Ideally, a mixer shall be
installed just upstream of the
sampling point to ensure the
liquid well mixed /
homogenous sample

Courtesy picture http://www.eesiflo.com/watercut-monitoring-mbw.html

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SAMPLING : SAMPLING POINT (2)

• If the end of sampling located at 6 o'clock direction, we

may only get the water, while the end of sampling point
located at 12 o'clock position we may get mostly crude
STRINGER oil or even gas.
• A tools called as stringer may help to get sample at each
position
• A stringer end point can be raised and lowered on the
pipe
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SAMPLING : QUALITY

Parameter
Representative of the production
system
Consistent with current production
Contaminant free (absence of
normally injected field chemicals)
Fresh
Remark
Sample taken from most of wells/manifold especially well
with high production or contribute to tight emulsion
The composition of sample similar with average field
production
Especially not contaminated with Corrosion Inhibitor
Sample not aging, some sample will decompose when
exposed to open air or after heating many times
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SAMPLING : QUANTITY

• A bottle tester shall calculate how many test will carried out from the pre-test, selection,
formulation, optimization include some spare.
• Some fields not easy to re-access and may only allow the bottle tester to only conduct
once of sampling such as at remote offshore area.
• For example if we will conduct 100 test @ 100 ml with oil:water composition 60:40 then
we shall has sample :
• Total sample = 100 test * 100 ml/test * 1.2 (as spare) = 12,000 ml sample
• Oil sample = 60% * 12,000 = 7,200 ml
• Water sample = 40% * 12,000 = 4,800 ml
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LABORATORY TEST

Ratio Intermediate
Synergy Formulation Optimization Stability
Test Screening
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REAGENT

• Toluene as light hydrocarbon solvent

• Incumbent demulsifier (if available)
• Fast Knock Out Demulsifier
• Series of Demulsifier
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EQUIPMENT

• Glass bottle • Thermometer

• Micropipette • Formulation bottle
• Syringe • Pipette drop
• Water bath • Stopwatch
• Shaker
• Centrifuge and Tube
 GLASS BOTTLE

Torpedo
Sanniglass Tube

Courtesy picture : https://amglassware.com/100ml-demulsifier-tube/

 WATERBATH

Courtesy picture : https://www.memmert.com/fileadmin/_processed_/csm_WPE45_Offen_85537fe8cd.png://amglassware.com/100ml-demulsifier-tube/

 SYRINGE AND
MICROPIPPET

Micropippet
Syringe
CENTRIFUGE AND CENTRIFUGE TUBE
 SHAKER

Courtesy picture : https://amglassware.com/100ml-demulsifier-tube/

OTHERS LABORATORY EQUIPMENT
Measuring
Cylinder

Dropping Thermometer
Pippette

Formulation
Bottle
Wash Bottle Stopwatch
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RATIO TEST

• Ratio test used to determine optimum initial incumbent

RATIO TEST demulsifier dosage
60
• Steps :
50
• Calculate the incumbent dosage in the field. For example
WATER DROP (ML)

40 X ppm
30 • Conduct the test with variation dosage 0 ppm (blank),
20 ¼X ppm, , ½X ppm, X ppm, 2X ppm
10 • Observe where bottle that has medium (not the lowest
0 or highest) water drop then determine as the initial
0 10 20 30 40 50 dosage.
DOSAGE (PPM)
• At graph beside, the ratio test is at 10 ppm
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INTERMEDIATE SCREENING

• Single component demulsifier called as intermediate.

• Intermediate could be mixed each other
• If we have a lot of intermediate, we may screening the. For example if we have
100 intermediate, we may select only 10-15 intermediate.
• The screening parameter could be the water drop, top cut, interface or water
quality depend on the determined KPI
• There are some mathematical method for the intermediate screening and this
could be propriety for each specialty chemicals company.
• From the screening we will have some potential component

Courtesy picture : https://www.crodaoilandgas.com/discovery-zone/functions/demulsifier-intermediates

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SYNERGY

Water Drop • When we mix one intermediate to another, we may found

Code BS&W (%) the performance increase more than prediction. This
(ml)
phenomenon called as synergy
24C 0.8 40
• See beside illustration :
33G 1.2 60 • 24C+33G have synergy in BS&W since it provide
45D 0.3 20 better BS&W compare to the single component
24C + 33G 0.5 50 • 24C+45D have synergy for both BS&W and water
drop
24C + 45D 0.1 60
• 33G+45D not compatible since the mixture provide
33G + 45D 1.5 10 worse performance in BS&W and water drop
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FORMULATION

• We may continue the demulsfier bottle test by combine the

synergy solution with another intermediate
• The demulsifier formulation may consist of 3 or more
intermediate
• More component may provide more stable demulsifier in term
of emulsion characteristic fluctuation but it may impact to raw
material stock.
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OPTIMIZATION

BS&W VS PPM • In this step, we try to find the optimum dosage of

demulsifer formula
2,5
• Demulsifier has overtreat effect. Above the optimum
2
dosage the performance stagnant or even decrease
1,5 Optimum
BS&W

Dosage • At beside graph, the optimum dosage is at 40 ppm

1
where the BS&W around 0.2%. At higher dosage (80
0,5 ppm and 160 ppm) the BS&W not decrease significantly
0 compare to dosage 40 ppm
0 50 100 150 200
PPM
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STABILITY AND CONSISTENCY

• Stability means the demulsifier formulation not separate after mixing. Demulsifer final
formula may contain intermediate with different basic compound. To review the stability,
we blend the larger volume of formula for example up to 1,000 ml and observe for 3-7
days. If separation found we may add co-solvent to stabilize, but not work we cannot use
the formula as final demulsifier
• Demulsifier formula shall show consistent performance when we repeat the bottle test.
For example if conduct the test on 2 May with result BS&W 0.2 and water drop 60 ml,
the result shall be relatively consistent when we repeat the test on the next day.
EXERCISE
FIELD CONDITION

Data Result

BFPD 13000
BOPD 1500
Injection Rate Demulsifier, gpd 8
Volume washtank, bbls 1000
Temperature washtank, OF 120
PLEASE DESIGN THE DEMULSIFIER BOTTLE TEST

?
Bony Budiman

CONCLUSION AND RECOMMENDATION

• Emulsion at each field is specific depends on crude and water composition, agitation,
temperature and emulsifying agent
• Demulsifier is a specialty chemicals. One demulsifier cannot work for all emulsion type
• Bottle test demulsifier is the best method to determine the suitable formula for each
field
• Need an extensive bottle tests at many fields to become an expert demulsifier bottle
testes
Bony Budiman

REFERENCES

• ASTM No D 4007-02 : “Standard Test Method for Water and Sediment in Crude Oil by
Centrifuge Method”
• https://www.crodaenergytechnologies.com/en-gb/functions/demulsifiers
• https://www.slideshare.net/ChandranUdumbasseri1/demulsifier-chemistry-and-rsn-
170715-50699603
• Demulsifiers-Specialty Oilfield Chemicals, Presentation by Chandran Udumbasseri,
Technical Consultant