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Oil Dispersion

Step-by-Step Guide

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TM
Oil Dispersion
A Step-by-Step Guide
Croda have created a simple, step-by-step guide to further your
understanding of Oil Dispersion (OD) formulations. This guide aims
to help conquer the frequent difficulties associated with formulating
ODs. We encourage you to contact our Crop Care experts with queries.
They are waiting to support you.

Step 1 - Select the Oil for Continuous Phase


Consider:
Solubility of active ingredient – The active ingredient (A.I.) must not be soluble in the selected oil to prevent
crystal growth.
Test for solubility of active ingredient: Observe if any of the active has been solubilised in the oil.
This could be by visual inspection or by HPLC. Microscopy can also be used to visualise any crystal
growth of the A.I.

4 PASS: The A.I. is not soluble


Move to step 2 8 FAIL: Select a different oil and re-do test Figure 1: Oil

Step 2 - Select the Type of Rheology Modifier

Consider:
Compatibility of rheology modifier with oil - It is important that the rheology modifier is able to provide and maintain
structure in the chosen oil.
Effect on the emulsifier system - Adding the rheology modifier at the end may destabilise the formulation and a new
emulsion system may have to be trialled. Incorporating the rheology modifier into the oil before selecting an emulsion
system, where possible, is highly beneficial (with the exception of Silica). If the inclusion level of rheology modifier is to be
increased, this may have a similar effect on the stability of the formulation.
Test for compatibility of rheology modifier and oil: Begin with a 5% w/w inclusion of rheology modifier in oil
(this is a high inclusion level but will give a good indication to whether the rheology modifier can provide structure). Figure 2: Oil & rheology modifier
The system should be a thickened oil which is readily flowable across the determined range of inclusion for the
rheology modifier. Once compatibility has been established, inclusion levels can be optimised later in development.
Note: Leaving at room temperature and 54 ºC for 24 hours to observe separation gives a good indication of
compatibility.

4 PASS: Move to step 3 8 FAIL: Select a different rheology modifier


Step 3 - Generate the Emulsifier & Non-aqueous Dispersant System
Consider:
Polarity of oil - The oil polarity can significantly impact the emulsion system required. Having a clear idea as
to the polarity of the oil gives a good starting point to selecting surfactant systems. A simple HLB test will give
an indication as to the polarity of the oil.
Note: Consider the emulsifier and non-aqueous dispersant together because the dispersant
may have co-emulsifier properties.
Test surfactant system with oil and rheology modifier - Perform CIPAC MT 36.3
Emulsifier
Non-aqueous dispersant

Figure 3: Oil, rheology modifier,


4 PASS: Move to step 4 8 FAIL: Try different surfactant system emulsifier and non-aqueous
dispersant

Step 4 - Prepare Oil Dispersion System


Add Active - Combine A.I. with selected oil, rheology modifier and surfactant system to produce the concentrate for dilution.
Note: Mill concentrate until desired particle size distribution (PSD) is achieved.

Consider:
Viscosity of system - A final formulation must remain readily flowable after the addition of the rheology modifier. If this is not the case, reduce
the rheology modifier inclusion level until flowability and stability are achieved.
Test Storage Stability - Perform CIPAC MT 46.3. Stability testing should be completed before fully formulating the system to avoid the
structure collapsing. Ensure there is enough rheology modifier to suspend the amount of active in the system. This is an empirical process;
if sediment is seen in the concentrate which is dispersible, it is likely that the level of rheology modifier needs increasing.
Test Dispersion Stability - Perform CIPAC MT 180

FAIL: Carry out analysis and troubleshooting


4 PASS: Move to outcome 1 8 as per outcomes 2-4 on the following page

Outcome 1 - Stable Emulsion upon Dispersion


On dilution

4 PASS: Congratulations!
Now progress to full
stability testing

Active ingredient stabilised


by non-aqueous dispersant
Emulsifier
Non-aqueous dispersant
Figure 5: Stable OD formulation on
Figure 4: OD concentrate dilution, no sedimentation, no creaming
Consider:
Position of the A.I. - If the result is not a stable emulsion after CIPAC MT 180, understanding of the LogP of the A.I. will help determine
the positioning of the active in the diluted formulation. Some common formulation instabilities are shown below.
Note: Once a formulation has been produced, using a microscope can highlight the positioning of the A.I. upon dilution in the oil droplet
or water phase. This gives a good idea as to how to overcome any issues which arise.

Outcome 2 - Creaming/Coalescence but No Sediment upon


Dispersion
This means A.I. is contained in the oil phase. Possible situations that may be occurring. 4 PASS: Congratulations!
Now progress to full
1. Too highly loaded
Note: Reduce A.I. loading stability testing

2. Active particle size too large, making emulsion droplets large


Note: Mill to desired PSD

3. Insufficient emulsifier in system


Note: Increase emulsifiers keeping the same ratio
8 FAIL: Re-assess,
adjust and re-test
Figure 6: Emulsion breakdown
mechanisms After adjustment perform CIPAC MT 180. CIPAC MT 180

Outcome 3 - Stable Emulsion but Fine, Redispersible Sediment


upon Dispersion
This means A.I. is in the aqueous phase. Non-aqueous dispersant is preventing For more information on how
flocculation but is unable to successfully disperse within water.
to formulate ODs and which
Note: Add aqueous dispersant. If selecting Atlox™
Metasperse 550S, add after milling to prevent products we recommend,
interference with particle size during milling process. visit our formulators tool
After adjustment perform CIPAC MT 180. box on our website
www.crodacropcare.com
Figure 7: Redispersible sediment or speak with your local
Croda representative.
Outcome 4 - Stable Emulsion but Sticky Sediment, Particles
Flocculating upon Dispersion
This means A.I. is in the aqueous phase. Non-aqueous dispersant lacks affinity for
A.I. causing particles to flocculate. Key
Note: Alter level/change non-aqueous dispersant in the Active ingredient
system. Consider adding an aqueous dispersant. Active ingredient stabilised
After adjustment perform CIPAC MT 180. by non-aqueous dispersant
Emulsifier
Non-aqueous dispersant

Oil droplet
Figure 8: Flocculation and sedimentation

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The information in this publication is believed to be accurate and is given in good faith, but no representation or warranty as to its completeness or accuracy is made. Suggestions for uses or applications are only
opinions. Users are responsible for determining the suitability of these products for their own particular purpose. No representation or warranty, expressed or implied, is made with respect to information or products
including, without limitation, warranties of merchantability, fitness for a particular purpose, non-infringement of any third party patent or other intellectual property rights including, without limit, copyright, trademark
and designs. Any trademarks identified herein are trademarks of the Croda group of companies.
©2018 Croda Europe Ltd 08/18 CCRG001v1 EN

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