Published on 07 February 2025
This application note describes oil-in-water droplet generation and coalescence analysis in petroleum samples, addressing challenges in emulsion stability studies. Utilizing Elveflow’s piezoelectric pump and advanced flow control technology, the custom microfluidic setup achieved precise droplet uniformity with size variations under 1%, critical for coalescence observations. Building on recent advances in 3D-printed microfluidic devices, the study integrates proprietary hydrophilic and solvent-resistant materials developed by Polaris. Developed in collaboration with the LC-GC research group at the Universidade Estadual de Campinas (Unicamp) and Petrobras, this approach combines high-resolution droplet generation and analytical techniques, offering a comprehensive solution to understand emulsion behavior, while showcasing Elveflow’s superior microfluidic flow control capabilities.
The developed microfluidic setup has broad applications in petroleum research, particularly in analyzing emulsion stability and coalescence phenomena. It can be utilized for studying oil recovery processes, optimizing demulsifier formulations, and investigating the impact of surfactants like naphthenic acids on emulsion behavior. Beyond petroleum, the system is versatile for assays in chemical engineering, environmental monitoring, and food sciences, where precise droplet generation and controlled flow conditions are critical. The integration of Elveflow’s advanced flow control and Polaris’ innovative materials further expands its potential in diverse research fields requiring high-resolution microfluidic analysis.
Microfluidic Device:
A custom-designed microfluidic device was fabricated using a novel polymer developed by Polaris. This material is hydrophilic, optically transparent, resistant to solvents such as toluene and xylene, and capable of achieving high-resolution channel geometries. The device incorporates a high-performance geometry tailored for passive coalescence of droplets without disrupting the laminar flow, enabling precise and efficient coalescence studies.
To replicate this microfluidic setup, the following instruments, consumables, and materials are required:
Elveflow OB1 MK4 microfluidic flow controller
Custom hydrophilic, solvent-resistant resin (developed by Polaris)
High-speed camera (e.g., Photron Fastcam S6)
Hexadecane (Sigma-Aldrich)
Inverted microscope (e.g., Nikon Ti-U Eclipse)
Ultrapure water (Millipore, 18.2 MΩ·cm)
External LED light source (e.g., HDF7010, Hayashi)
Technical mixture of naphthenic acids (Sigma-Aldrich)
3D printer (e.g., Phrozen Mini 4K)
Saline water samples with specified compositions
Anycubic Wash and Cure Plus machine
Demulsifier (20% w/w)
Flow sensor (e.g., MFS2, Elveflow)
HPLC-grade solvents (e.g., isopropanol, ethanol, dichloromethane, acetone, methanol)
Pressure sensors (e.g., MPS, Elveflow)
Sodium sulfate (anhydrous)
Rotary evaporator
Other Materials:
This setup leverages the unique properties of the Polaris-developed polymer and advanced flow control systems, providing a robust platform for oil-in-water emulsion studies and coalescence analysis.
Figure 1 : Microfluidic chip specifications. The device has three regions: A, B, and C. Region A corresponds to droplet generation, while regions B and C represent the first and second observation chambers, respectively. The histograms show the relative frequency of particles as a function of the equivalent diameter (µm) for these three regions. In histogram C, the coalescence of some droplets can be observed.
The integration of advanced imaging and analysis tools ensures a deep understanding of the coalescence process and its relationship to surfactant properties in petroleum samples
Figure 1 : Experimental setup with the Elveflow OB1 MK4 system. The setup integrates the Elveflow OB1 MK4 for precise flow control, a 3D-printed microfluidic device, a Photron Fastcam S6 high-speed camera, and an inverted microscope for real-time analysis of droplet generation and coalescence.
The setup operates by precisely controlling the flow of fluids through a custom-designed 3D-printed microfluidic device using the Elveflow OB1 MK4 system. A continuous phase (water) and a segmented phase (oil) are independently pressurized and delivered into the microfluidic device, where they intersect at a flow-focusing region to generate uniform oil-in-water droplets.
The high-resolution channels in the microfluidic device are optimized for passive coalescence, maintaining laminar flow conditions. Droplets move through serpentine channels and visualization chambers, where interactions and coalescence are observed. The system allows for real-time monitoring of droplet formation and coalescence using a Photron Fastcam S6 high-speed camera connected to an inverted microscope.
Captured videos are analyzed with custom software to extract key parameters such as droplet size distribution, coalescence time, and film rupture events. This approach ensures a detailed understanding of emulsion stability and the dynamics of coalescence (see video below).
Step 1: Prepare the Microfluidic Device
Step 2: Assemble the System
Step 3: Set Up the Fluids
Step 4: Adjust the Observation System
Step 5: Start Droplet Generation
Step 6: Record and Analyze
Step 7: Troubleshooting
Figure 2 : (Left) Droplet analysis software interface, Displays droplet size, coalescence time, and film rupture dynamics with real-time visualization and data extraction tools. (Right) Coalescence phenomenon observed in the microfluidic device. Sequence showing droplet coalescence with film rupture occurring within 0.9 ms, highlighting the system’s ability to capture rapid dynamics.
This research showcased how a custom microfluidic setup enables high-precision analysis of oil-in-water emulsions and coalescence phenomena. Key findings from the study include:
Microfluidics offers significant potential for improving the understanding of emulsion stability and coalescence phenomena in complex fluid systems. In this study, a custom 3D-printed microfluidic device—fabricated from a proprietary hydrophilic and solvent-resistant polymer—was combined with Elveflow’s precise flow control system to generate highly uniform droplets with size variations below 1%. This level of precision allowed for detailed observations of coalescence dynamics, including film rupture within 0.9 ms, shedding light on the influence of surfactants like naphthenic acids in emulsion behavior.
The results can guide the optimization of emulsion stabilization strategies, development of demulsifiers, and enhancement of oil recovery processes. The integration of advanced microfluidics and analytical techniques paves the way for innovations in emulsion-based systems across diverse industries.
We gratefully acknowledge the financial support provided by Petróleo Brasileiro S.A. (Petrobras), whose resources were instrumental in the success of this research. Petrobras, through its research and development center (CENPES), has been at the forefront of advancing knowledge and technologies in the petroleum industry. For more information, visit Petrobras R&D.
We also extend our thanks to the LC-GC Group at the Universidade Estadual de Campinas (Unicamp) for their collaborative efforts and technical expertise. This group specializes in advanced chromatographic and spectrometric techniques applied to complex mixtures, fostering innovations in analytical chemistry. Learn more about their work at Unicamp LC-GC Group.
Additionally, Polaris Microsystems & Nanotechnology extends heartfelt thanks to Elveflow for their exceptional support and partnership throughout this research. Their advanced flow control systems were instrumental in achieving the precision and reliability required for our experiments. Over the years, this collaboration has grown into a valued friendship, and we deeply appreciate their unwavering commitment to innovation and excellence.
Written and reviewed by Dr. Reverson Fernandes Quero and Louise Fournier, PhD. For more content about microfluidics, you can have a look here.
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