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NSF I/URC FOR PARTICULATE & SURFACTANT SYSTEMS Value with synergy between the sites strengths: NSF I/URC FOR PARTICULATE & SURFACTANT SYSTEMS Value with synergy between the sites strengths: Particles + Surface Active Agents Center Mission, Capabilities, Project Status & Highlights Brij M. Moudgil and P. Somasundaran, Co-Directors Industrial Advisory Board Meeting Columbia University, NY August 20, 2009

Center Mission To develop and advance fundamental understanding of particulate/surfactant systems for enhanced performance Center Mission To develop and advance fundamental understanding of particulate/surfactant systems for enhanced performance & minimal environmental footprint. This mission will be accomplished by achieving the following goals: Ø Advancing the fundamental understanding of the particulate-surfactant interactions for optimal performance in industrial applications (e. g. , consumer goods and advance materials and commodity industries); Ø Exploring high-risk, high impact research that could lead to technological innovations; Ø Establishing a venue for industrial-academic interactions for conducting industrially relevant research; Ø Promoting education and training of students in this important field

Project Presentation and Progress Review Spring IAB meeting (UF): Project Presentations and Selection Fall Project Presentation and Progress Review Spring IAB meeting (UF): Project Presentations and Selection Fall IAB meeting (CU): Project Progress Review • Joint Projects (UF & Columbia) Project themes (IAB members) Project ideas (Faculty researchers) • ~ 50 % fund: high impact/high risk type ideas • In future, the current 2 IAB programs will transition to a single IAB program Proposal (Researchers) Member IP Rights Review (IAB members) All IAB members including affiliates will vote on the proposed projects • Company may be granted an option to a royalty-free non-exclusive license

- Membership Benefits • Student & Post doc mentoring > Joint publications & patents - Membership Benefits • Student & Post doc mentoring > Joint publications & patents • Priority access to the Center’s infrastructure and facilities • First access to innovations developed with CPa. SS funding • Voting and Participation on biannual IAB Meetings • Enhanced joint funding opportunities • Direct communication with the faculty of the Center • Hiring opportunities among trained students from CPa. SS • Access to the PERC-CPa. SS Newsletter (industry ‘corner’)

Capabilities & Highlights - Columbia University - Looking back & Looking forward Capabilities & Highlights - Columbia University - Looking back & Looking forward

New and Continuing Industrial Advisory Board Members Paid Members Akzo-Nobel Church and Dwight CBET New and Continuing Industrial Advisory Board Members Paid Members Akzo-Nobel Church and Dwight CBET Systems/NSF Cognis Vale. Inco Cytec Industries Dial Dispersion Tech Elkay Chemicals Evonik Johnson & Johnson Modular* Newmont Gold. Unilever Tata/TRDDC In-Kind: Modular, Cytec, Vale. Inco, Newmont, Elkay, DT, Unilever Potential: Croda, ISP, Ciba Specialty Chemicals, Hercules, Cabot, SC Johnson. . *New

Columbia Surfactant/Particles Team Charles Maldarelli Somasundaran Nick Turro Larry Chasin Paul Duby Interfacial Fluid Columbia Surfactant/Particles Team Charles Maldarelli Somasundaran Nick Turro Larry Chasin Paul Duby Interfacial Fluid Mechanics Adsorption Dispersion Biosurfaces Photoluminescence Microbiology Electrodeposition External Collaborators F. Ottaviani Italy ESR Pradip/Venkat India Polymer/particulate interactions D. R. Nagaraj Cytec Mineral process/separation R. D. Kulkarni Pune Fabric modification & care J. Lee CUNY Gas hydrates R. Gross Brooklyn Biosurfactants T. Healy Australia Colloidal rheology D. Mac. Donald Bronx VA Hospital I. Nambi Chennai Microbial surfactants CEIN (NSF/EPA Center for Environmental Implications of Nanotech), U. Florida

Scientific Instrumentation Available to IAB Members REAGENT PARTICLE CHARACTERIZATION Analytical Ultracentrifuge UV-Vis, HPLC, NMR Scientific Instrumentation Available to IAB Members REAGENT PARTICLE CHARACTERIZATION Analytical Ultracentrifuge UV-Vis, HPLC, NMR Mass. Spec. , TGA, micro GC, ICP, SURFACE ACTIVITY Liq/Liq extraction, Acoustophoresis, PCS, Surface area, Streaming potential, SEM-EDX, Centrifugal Immersion, Levitation, Flotation, CA, Surface tension, TOC INTERFACIAL & COLLOID NANOSTRUCTURE AFM, QCM, Fluorescence, ESR, FTIR, XPS, Raman* Rheometer Microtrac Electrophoresis, Uncommon techniques: Analytical Ultracentrifuge – surfactant aggregates & polymer species distribution Surface Plasmon Resonance – dynamics of interactions, short-term and long-term Life Time/Steady State Fluorescence + ESR - Colloidal/interfacial nanostructures Cluster computing - abinitio modeling/simulation of NPs surface properties

Analytical Ultracentrifuge for Monitoring Micellar Distribution Single and mixed micelles: Size, Shape, Aggregation number Analytical Ultracentrifuge for Monitoring Micellar Distribution Single and mixed micelles: Size, Shape, Aggregation number T. Sobisch and D. Lerche. WPT Conf, May 2006

DYNAMICS – Challenge is to Monitor and Control Stage 1 Convective-Diffusive Kinetics Stage II DYNAMICS – Challenge is to Monitor and Control Stage 1 Convective-Diffusive Kinetics Stage II -Rate lowered Stage III - Rate increased

Recent Research Project Highlights - Columbia Site Mixed surfactants: Synergy in surface tension, Hydrophobicity, Recent Research Project Highlights - Columbia Site Mixed surfactants: Synergy in surface tension, Hydrophobicity, Viscoelasticity, (Type, Ratio) Green Surfactants (Glucosides, Lipopeptides, Acyl Glutamides): High surface activity, Synergy, Selective adsorption Polymer/Protein/Surfactant/salt: Coarsevation > solubilization > reprecipitation > solubilization (Ratio, Sequence) Silicones: Functionalization, Concentration > Surface Pressure, Smoothness, Friction Vesicles, Liposomes, Nanogels particles: Controlled Extraction, Release, Tissue engineering Corrosion/wear/ inhibition/Imaging: Inhibitor charge type, dosage, Lubricant chemistry Fines/Fibers in mineral dispersion and separation: Aspect ratio, Volume % Nanoparticles: Effect of size, morphology, Toxicity

New Developments *TIE grant to collaborate with IIT Madras on Biosurfactants: 50 K • New Developments *TIE grant to collaborate with IIT Madras on Biosurfactants: 50 K • NSF Exploratory Research Grants: 75 K/Center *NSF/EPAC for Environ. Implications of Nanotech: ~$450 K/4 years *NSF Equipment grant for Raman microscope: 70 K *Nature article reference: Nanobio interface, July 2009 *J Phys Chem Cover article on spec probing of liposomes for controlled efficient delivery, January 2009 *Olympics in Surface Science at Columbia: 13 th International Conference of Surface and Colloid Science& 83 rd ACS National Surface & Colloid Science June 14 -18, 2009 1400 participants, 1300 papers, 40 Countries www. icscs. org

Nanotoxicity of Anatase Particles on N. Europaea a b c d N. Europaea cells Nanotoxicity of Anatase Particles on N. Europaea a b c d N. Europaea cells in media containing a) control (no anatase Ti. O 2 nanoparticles (NPs)), b) 20 ppm of 25 nm anatase Ti. O 2 NPs c) 200 ppm of 25 nm anatase Ti. O 2 NPs, d) 200 ppm of 200 nm anatase Ti. O 2 NPs for 4 hours.

The Properties of Nanoparticle Related with Nanotoxicity 4 3 M n+ 1 9 8 The Properties of Nanoparticle Related with Nanotoxicity 4 3 M n+ 1 9 8 7 5 3 2 ROS 6 10 O 2 / H 2 O 1. Morphology-aspect ratio/size 2. Hydrophobicity 3. Surface area-roughness/porosity 4. Solubility-release of toxic species 5. Surface speciescontaminations/adsorption during synthesis/history 6. Capacity to produce ROS 7. Structure/composition 8. Surface charge 9. Competitive binding sites with receptor 10. Dispersion/aggregation

Vibrational Spectroscopy : Raman and IR Molecular Vibrations Wavelength 3 -20 m virtual electronic Vibrational Spectroscopy : Raman and IR Molecular Vibrations Wavelength 3 -20 m virtual electronic states vibrational states jchemed. chem. wisc. edu § accessible, § non-invasive, § real time (time resolution up to 10 -3 sec) § in situ, § in vitro/in vivo § a lot of information

Surface Activity of Modular Acyl Glutamate Ajinomoto Myristoyl Glutamate ■ ● Myristoyl Glutamate MG Surface Activity of Modular Acyl Glutamate Ajinomoto Myristoyl Glutamate ■ ● Myristoyl Glutamate MG Acyl Glutamate shows higher surface activity vs Commercial 16

Problems and Challenges: Structure-Property-Performance Relationships Optimum structure: Predictability of Synergy in Wettability, Concentrated dispersions, Problems and Challenges: Structure-Property-Performance Relationships Optimum structure: Predictability of Synergy in Wettability, Concentrated dispersions, Surface Softness Desired Dynamics: Short/Long Term Real-time response to perturbation Nanoparticles: Surface effects, Nanotoxicity Rheology control: Fine Particle Processing Delivery of Actives: Complex fluids Greener reagents: Synergy, Biodegradation, Recyclability, Non-toxic

2009 -2010 Program Highlights - Florida Site - 2009 -2010 Program Highlights - Florida Site -

Florida Site Industry Members (CPa. SS) Florida Site Industry Members (CPa. SS)

Florida Site In-Kind Members (CPa. SS) Florida Site In-Kind Members (CPa. SS)

Project Selection at Florida The voting process held last April/May resulted on the selection Project Selection at Florida The voting process held last April/May resulted on the selection of the following projects at Florida: 1. Dilute Suspension Flow- An experimental and Modeling Study. Jennifer Curtis 2. Triboelectric Phenomena in Particulate Materials- Scott Brown 3. Grinding Aids for Nano-Milling using Stirred Media Mill. Parvesh Sharma 4. Particle-Process Analytical Technology (P-PAT)- Kevin Powers 5. Photocatalytic Degradation of Microbes – Vijay Krishna 6. Sampling- Theory and Practice, Part I- Dry Powders [emodule]- Hassan El-Shall 7. Dispersion in Air of Micron and Nanometer Sized Particulate Systems- Hassan El-Shall, Nate Stevens NEW NSF supplementary grant: Α fundamental study of nanoparticle – protein mutual interactions: Role of nanoparticle morphology, Georgios Pyrgiotakis ( UF) & Irina Chernyshova (Columbia)

Facilities and Equipment • Particle Properties: • 25+ methods for Particle Size Analysis • Facilities and Equipment • Particle Properties: • 25+ methods for Particle Size Analysis • 4 methods for Zeta Potential • Density/Surface Area • SEM/TEM/AFM/(Confocal) • UV-Vis/FTIR/FTNIR/Raman • Elemental and Surface Analysis • Mechanical and Physical (6 Powder mechanics testers) • Particle Processing: • Classification • Comminution • Mixing/Blending • Particle Synthesis • Rheology • Spray Drying (new) • Fluid Bed Drying (new) • Particle Coating Particle Characterization is more than just Equipment! CRIT Personnel/Scientists/Engineers Gill Brubaker - MS Physics – Senior Technician Gary Scheiffele - BS Ch, over 20 years Experience Kerry Siebein – MS Materials STEMZ/FESEM

Recently Added Processing Capabilities Niro Mobile Minor. TM Spray Dryer Retsch Water Jet Sieve Recently Added Processing Capabilities Niro Mobile Minor. TM Spray Dryer Retsch Water Jet Sieve Retsch Fluid Dryer Roll Mill (donated by Du. Pont) Hockmeyer Stirred Mill Union Process Stirred Media Mill

What’s Unique / New Instrumentation at UF • Leading technique to analyze mixtures of What’s Unique / New Instrumentation at UF • Leading technique to analyze mixtures of NMs, including SWCNTs, quantum dots, or nanocrystals. • Optimized for detecting nanomaterials’ near-IR fluorescence. Nano. Log Spectrofluorometer for Nanomaterials Capabilities: – Measure quantum yields – Real time phosphorescence – Quantify free radicals

Technology Vision Developing a fundamental framework for smart, multifunctional particulate systems —a ‘nano-bio toolbox’ Technology Vision Developing a fundamental framework for smart, multifunctional particulate systems —a ‘nano-bio toolbox’ from fundamentals to applications Nanoscale Coatings for Enhanced Drug Delivery Key Collaborators: Guenther Hochhaus 1, Rajiv Singh 2 (Pharmacy 1& Materials Science and Engineering 2) Developed pulsed laser ablation technology for nanoscale sustained-release drug delivery coatings Spin-off Company Nanotherapeutics, Inc.

Imaging and Cancer Therapy in a Single Particle Key Collaborators: S. Grobmyer 1, Huabei Imaging and Cancer Therapy in a Single Particle Key Collaborators: S. Grobmyer 1, Huabei Jiang 2 (Surgical Oncology 1, Biomedical Engineering 2) Developing novel multifunctional contrast agents Non-invasive bioimaging = (PAT, MR and Fluorescence) + Capable of photothermal ablation (NIR absorbing) Selective ablation of lung cancer cells Dead cells stained blue

Nanotoxicology: Insights into Nano-Bio Interactions Key Collaborators: Steve Roberts 1, David Barber 1, Nancy Nanotoxicology: Insights into Nano-Bio Interactions Key Collaborators: Steve Roberts 1, David Barber 1, Nancy Denslow 1, Luis Garcia-Rubio 2, (Vet. Med. 1, Claro Sci 2) • Raman investigates the chemical composition of the cells • Multiangle-multispectral analysis: Changes in cell morphology • Combination of two technologies: More definitive assessment Broad-based program to understand the environmental and human implications of nanomaterials Realtime Non-invasive Intracellular Monitoring

Drying for Green Manufacturing Key Collaborator: Arun Ranade (Particle Technologies, LLC) Ø Drying an Drying for Green Manufacturing Key Collaborator: Arun Ranade (Particle Technologies, LLC) Ø Drying an important unit operation in particulate processes Ø Energy-efficiency and Green-manufacturing is pivotal for sustainability Ø New drying strategies required for achieving sustainability Time Required for Drying (Hours) Performance Assessment for Aluminum Flakes Supercritical drying an optimal solution!

Outcomes & Future Endeavors Last One Year 5 2 Peer Reviewed Journal Articles 10 Outcomes & Future Endeavors Last One Year 5 2 Peer Reviewed Journal Articles 10 International & National Conference Presentations Interdisciplinary Grant Applications Submitted (1 Awarded) (NSF, NIH, Keck) Near Term Focus Highlight green aspects of on-going and future Florida projects Long Term Goal Computational methods based engineering of green particulate systems

Acknowledgements • CPa. SS Industry Members - Florida and Columbia Sites -NSF (I/UCRC Program) Acknowledgements • CPa. SS Industry Members - Florida and Columbia Sites -NSF (I/UCRC Program)