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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