Wang Haoyu, Khodaparast Sepideh, Carroll John, Kelly Caroline, Robles Eric S J, Cabral João T
Department of Chemical Engineering, Imperial College London, London SW7 2AZ, United Kingdom.
National Formulation Centre, Centre for Process Innovation, Sedgefield DL1 1GL, United Kingdom.
Rev Sci Instrum. 2020 Apr 1;91(4):045109. doi: 10.1063/1.5144770.
Measurement of the phase behavior and (meta)stability of liquid formulations, including surfactant solutions, is required for the understanding of mixture thermodynamics, as well as their practical utilization. We report a microfluidic platform with a stepped temperature profile, imposed by a dual Peltier module, connected to an automated multiwell plate injector and optical setup, for rapid solution phase mapping. The measurement protocol is defined by the temperature step ΔT ≡ T - T (≲100 °C), volumetric flow rate Q ≡ ΔV/Δt (≲50 μl/min), which implicitly set the thermal gradient ΔT/Δt (≃0.1-50 °C/min), and measurement time (which must exceed the intrinsic timescale of the relevant phase transformation). Furthermore, U-shaped microchannels can assess the reversibility of such transformations, yielding a facile measurement of the metastable zone width of the phase diagram. By contrast with traditional approaches, the platform precisely controls the cooling and heating rates by tuning the flow rate, and the absolute temperature excursion by the hot and cold thermal profile, which remain stationary during operation, thus allowing the sequential and reproducible screening of large sample arrays. As a model system, we examined the transition from the micellar (L) to the liquid crystalline lamellar phase (L), upon cooling, of aqueous solutions of sodium linear alkylbenzene sulfonate, a biodegradable anionic surfactant extensively employed in industry. Our findings are validated with quiescent optical microscopy and small angle neutron scattering data.
为了理解混合热力学及其实际应用,需要测量包括表面活性剂溶液在内的液体制剂的相行为和(亚)稳定性。我们报告了一种微流控平台,它具有由双珀耳帖模块施加的阶梯式温度分布,连接到自动多孔板注射器和光学装置,用于快速溶液相映射。测量协议由温度步长ΔT≡T - T(≲100°C)、体积流速Q≡ΔV/Δt(≲50μl/min)定义,这隐含地设定了热梯度ΔT/Δt(≃0.1 - 50°C/min)以及测量时间(必须超过相关相变的固有时间尺度)。此外,U形微通道可以评估此类转变的可逆性,从而轻松测量相图的亚稳区宽度。与传统方法相比,该平台通过调节流速精确控制冷却和加热速率,并通过热冷温度分布精确控制绝对温度偏移,在操作过程中热冷温度分布保持不变,从而允许对大量样品阵列进行顺序且可重复的筛选。作为一个模型系统,我们研究了线性烷基苯磺酸钠水溶液在冷却时从胶束相(L)到液晶层状相(L)的转变,线性烷基苯磺酸钠是一种在工业中广泛使用的可生物降解阴离子表面活性剂。我们的研究结果通过静态光学显微镜和小角中子散射数据得到了验证。