Abstract:
The dataset contains spreadsheet data, optical micrographs and cryo-electron micrographs of the application of halloysite-magnetic iron oxide nanocomposite oil emulsification and mobilization. Transmission electron microscopy and thermogravimetric analysis were used to show successful loading of surfactant into magnetically functionalized halloysite clay nanotubules (MHNT). Additional data reported include the droplet diameter and stability of emulsions prepared with various MHNT concentrations. This data supports the paper “Interfacial adsorption and surfactant release characteristics of magnetically functionalized halloysite nanotubes for responsive emulsions" published in Journal of Colloid and Interface Science doi:10.1016/j.jcis".
Suggested Citation:
Vijay John, Olasehinde Owoseni. 2016. Dataset for: Interfacial Adsorption and Surfactant Release Characteristics of Magnetically Functionalized Halloysite Nanotubes for Responsive Emulsions. Distributed by: GRIIDC, Harte Research Institute, Texas A&M University–Corpus Christi. doi:10.7266/N7M906MN
Purpose:
Our objective in this work is to encapsulate surfactants representative of COREXIT 9500, the commonly used dispersant in oil spill remediation, into the tubular voids of magnetically responsive halloysite. We show that magnetic clay tubules stabilizes oil-in-water emulsions, makes oil magnetically responsive and releases the surfactants for optimal oil dispersion.
Data Parameters and Units:
Figure 1a-d: image data from scanning electron microscopy of native (a and b) and magnetite (c and d) halloysite nanotubes (HNT) (SEM voltage 3kV and working distance = 8 mm); Figure 1e-f: Image data from transmission electron microscopy (TEM voltage 300 kV); Figure 1f E: TEM electron diffraction pattern of crystalline iron oxide nanoparticles Figure 1g Energy-dispersive X-ray spectroscopy (EDS) spectrum of magnetite HNT (M-HNT); Figure 2a XRD HALL AND MAG.xslx: 2Theta angle (degrees), Intensity (a.u.); Figure 2 b magnetic responsiveness.jpg – photograph of magnetic responsiveness of M-HNT powder to a 7 mT bar magnet; Figure 2b Magnetization Curve.xlsx: Applied Field (Oe), Magnetization (emu/g); Figure 3 inset optical microscopy images of emulsion at 0.01 wtpercent MHNT and 0.1 wtpercent HNT.jpg: optical microscope images of emulsions stabilized by 0.01 wt% and 0.1 wt% M-HNT(magnification used for optical microscopy in figure 3a and 3b was 10x/0.30 on a Nikon Eclipse LV100 Microscope); Figure 3b magnetic mobilization a-d.jpg; photographs of magnetic responsiveness of 1% wt M-HNT in water emulsion on a glass slide (volume = 200uL) to a 7 mT magnet; Figure 3 Fraction of oil resolve on centrifugation for dodecane-in-water emulsions.xlsx: particle concentration (wt%) and fraction of oil resolved in centrifugation (columns b and c are replicates). Figure 4a Cryo SEM images of magnetic HNT stabilized emulsion.jpg: cryo-scanning electron microscope image of dodecane-in-water emulsion (SEM voltage 3kV, working distance 8 mm); Figure 4a Photograph of magnetic HNT stabilized emulsion.jpg – photograph of a vial contain magnetic HNT stabilized emulsion; Figure 4b – 4d.jpg cryo-scanning electron microscopy images of dodecane-in-water emulsion (SEM voltage 3kV, working distance 8 mm), Figure 4a is a low resolution image, Figure 4b shows one of the oil droplets from figure 4a at a higher resolution, Figure 4c and 4d are high resolution images taken at two different points on the interface of the droplet in Figure 4b, (magnification used for SEM images 4a, 4b, 4c, 4d are 80x, 1000x, 30000x and 35000x respectively) ; Figure 5a-b: SEM (a) and TEM (b) scanning and transmission electron microscopy images of M-HNT loaded with 11.31 wt% Tween 80 (TEM voltage = 300 kV), (magnification used for image 5a is 40000x); Figure 6a TGA Data.xlsx: thermogravimetric data of curves of M-HNT with various Surfactant type (DOSS, Tween 80) and loading (wt%), temperature (degrees Celsius), Mass loss (%); Figure 6b DTA Data.xlsx: differential thermal analysis data for M-HNT loaded with different levels of DOSS, Surfactant loading (wt%), temperature (degrees Celsius), Mass loss per temperature change (dm/dt, a.u), Figure 7a-f optical microscopy images of emulsions stabilized at 0.1 wt% M-HNT and 0.1 HNT with various surfactant loadings of (a) 0wt%, (b) 1.5wt% dioctyl sulfosuccinate sodium salt (DOSS), (c) 4.05 wt% DOSS, (d) 9.63wt% DOSS, (e) 3.96wt% Tween80, (f) 7.86wt% DOSS-Tween 80 at ratio of 60:40 (magnification used for optical microscopy in figure 7a – 7f was 10x/0.30 on a Nikon Eclipse LV100 Microscope); Figure 8a-d cryo-scanning electron microscopy imaging of dodecane in water emulsion stabilized by DOSS loaded MHNT where concentration M-HNT is 0.7wt% and DOSS loading in M-HNT is 9.63% (magnification used for SEM images 8a, 8b, 8c, 8d are 70x, 2000x, 100000x and 120000x respectively); Figure 8e Dynamic Interfacial Tension.xlsx: Tween 80 l and DOSS loading in magnetic halloysite (Time (s), interfacial tension (mN/m) , Figure 9 : droplet number, particle size (micron) of emulsions stabilized by M-HNT and 1.5% DOSS, 4.05% DOSS, and 9.63%DOSS immediately after preparation and after 5 weeks;
Methods:
Emulsion Preparation: The nanotubes were uniformly dispersed in water by ultrasonication (Cole-parmer 8890) for 1 minute. Dodecane was then added to the nanotube dispersion at a dodecane to water ratio of 1:3. The emulsions were then prepared by vortex mixing at 3000rpm (Thermolyne Maxi Mix II) for 2 min. Optical Microsscopy: A small aliquot of the oil-in-water emulsion was removed using a Pasteur pipet and diluted with water prior to imaging on a Leica DMI REZ optical microscope. The images were analyzed using Image ProPlus v. 5.0 software to obtain the droplet sizes. Cryo-Scanning Electron Microsocopy: The structure of drop interfaces were imaged by Cryo-scanning electron microscopy (Cryo-SEM) imaging on a Hitachi S-4800 field emission Scanning Electron Microscope operated at a voltage of 3 kV and a working distance of 9 mm. The emulsion sample was first plunged into liquid nitrogen, followed by fracturing at −130 °C using a flat-edge cold knife and sublimation of the solvent at −95 °C for 5 min. The sample was sputtered with a gold–palladium composite at 10 mA for 88 s before imaging.
Instruments:
scanning and cryo-scanning electron microscopy (Hitachi S-4800 field emission Scanning Electron Microscope), optical microscopy (Leica DMI REZ optical microscope), and transmission electron microscopy (TEM) imaging using a FEI Tecnai G2 F30 Twin Transmission Electron Microscope
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