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Interfacial rheology

An interface is the contact area of two immiscible phases (e.g. water/oil-interface). The Interfacial Rheology System (IRS) is used to measure the rheological properties of an interfacial layer between two liquids or between a liquid and a gas (air). It allows the study of the effects of different surfactants on the stability of the layer (e.g. the formulation of emulsions or foams, or the stability of droplets) and enables rheological measurements of the weakest interfacial structures.

Background

Figure 1: Bi-cone above the IRS

The IRS combined with an MCR rheometer permits so-called two-dimensional rheological measurements of interfacial films at the air/liquid and liquid/liquid interfaces.

For these measurements, the shear stress becomes the interfacial shear stress τs  in [τs] = Pa·m. The viscosity turns to an interfacial shear viscosity ηs with the relationship: τs = ηs ·γ . The interfacial shear viscosity is measured in [ηs] = Pa·s·m = N·s/m or surface Poise.

A specific measuring system (e.g. bi-cone – see following figures) is placed at the interface and measures absorbed or spread films, e.g. films produced by proteins or surfactants.

Please note: Interfacial shear rheology only makes sense if a film is present!

There are two general methods to create interfacial films: spreading or absorbing.

Spreaded films (mainly for low-molecular-weight surfactants), which can be created by:

  • dissolving in a spreading solvent (e.g. hexane, ethanol, chloroform)
  • spreading directly onto the water with a micro-syringe
  • waiting for complete evaporation of the solvent
  • pouring the oil phase on top of the surfactant film

Absorbed films (e.g. for interfacial layers of protein), which are created by absorption from the bulk phase to the interface. This can be achieved by:

  • dissolving the proteins in distilled water
  • pouring the oil phase gently on top of the water/protein solution

Figure 2: measurement option of the IRS

The IRS, as a combination of MCR and bi-cone geometry, enables the rheological measurements of the weakest interfacial structures. Additionally, with a bi-cone geometry, high interfacial viscosities can be measured.

Raw data is produced by well-known rheological standard tests, and the interfacial properties can then be calculated by analyzing it. A post-processing hydrodynamic-flow-field analysis subtracts the contribution of the bulk and covering phase and calculates the relevant interfacial properties of the measured interfacial layer. Measurements can be performed in rotational and oscillatory modes, e.g. allowing flow curves and creep tests at an interfacial layer or oscillatory tests during film-formation processes.

The temperature is controlled by Peltier elements in the range from 5 °C to 70 °C; the patented normal force sensor in the air bearing of the MCR rheometer allows the accurate positioning of the bi-cone in the interface.

Typical tests that can be performed are:

  • Time tests to follow interfacial film formation
  • Flow curves
  • Amplitude sweeps
  • Frequency sweeps

Typical applications:

  • Food: emulsions and foams
  • Consumer products: emulsions, foams, and surfactants
  • Pharmaceuticals: encapsulation and drug release
  • Oil industries: surfactants, drag reducer, and water-oil systems
  • Langmuir monolayers: films at the water-air interface

Measurement example

The following figure illustrates a representative measurement investigating interfacial rheological properties of coffee crema. It shows the film formation for the same coffee sample at three different concentrations. When measuring at constant strain and constant frequency, it is possible to follow the adsorption and network formation of the surface-active ingredients at the liquid/air interface. For higher concentrations, the film shows elasticity already after a shorter time. In the case of the lowest concentration, the moduli increase over a longer time and still haven’t reached plateau values at the end of the experiment. This indicates that the higher the concentration of the coffee powder, the faster the film formation. 

Figure 3: Film formation of coffee samples at different concentrations: 0.05 g (blue curves), 0.15 g (green curves), and 0.3 g (red curves) of coffee powder in 114 mL double-distilled water.

Find more details in the application report: Interfacial shear rheology of coffee