This NSF PREM consist on the partnership of four institutions that complete the PREM pathway: Two primarily undergraduate institutions (PUI), Universidad Ana G. Méndez Cupey Campus and Gurabo Campus, which have more than 99% of Hispanic students (Recruitment and Retention); the University of Puerto Rico – Río Piedras, a Hispanic-serving and Doctorate Intensive Institution by the Carnegie Council (Recruitment, Retention, and Degree attainment); the Cornell High Energy Synchrotron Source (CHESS), a DMR-supported center (Retention and Degree attainment).

Cornell High Energy Synchrotron Source (CHESS)

The CHESS Center (J. Brock, Director) X-ray activity itself consists of two divisions: (1) The central division on which the other divisions depend is the NSF-DMR supported CHESS National Facility (J. Brock, PI, and M. Miller and E. Fontes, Associate Directors). Some support also comes from NIH-NIGMS via interagency transfer to NSF-DMR. (2)  NIH-NIGMS supports the MacCHESS Research Resource (R. Cerione, PI, M. Szebenyi, Director), which assists macromolecular crystallography users at CHESS.

Internal Physical and Personnel Resources

Laboratory Space

Net assigned sq. ft: Wilson Laboratory: 71,150; Wilson Annex: 8,890; Wilson Lab Modular Space: 8,880; Newman Laboratory (2 connected buildings): 34,000 sq. ft.; JBC (rented warehouse space): 14,400 sq. ft.

The research group supported under this grant has available to it the full facilities of the Wilson/Newman Labs complex at Cornell University. CHESS, the NSF supported National User Facility, and CESRTA, are both part of this complex. The Wilson/Newman complex is a set of fully self-contained, major accelerator physics and synchrotron radiation national facilities, including the full complement of metal, electronic, vacuum, chemical, and computer shops and stockrooms. Additional shop facilities of practically any type required are available as part of Cornell’s system of research facilities. These include the Cornell National Nanofabrication Facility and materials characterization facilities at the Cornell Center for Materials Research (described below).

An additional 3000 sq. ft. of research space in Clark Hall houses the Cornell X-ray detector development group, which is under Prof. S. Gruner’s direction and largely independently funded. This capability includes a full set of the computer tools to perform Pixel Array Detector (PAD) integrated circuit design, simulation and testing; equipment required to test custom analog and digital detector PAD integrated circuits, clean laminar flow hoods, dark boxes equipped for PAD diode testing, and X-ray generators and beamline equipment for X-ray testing and calibration of detectors. Most importantly, the laboratory is staffed by professional personnel who are highly experienced in all aspects of X-ray detector design, fabrication, and assembly. A recent accomplishment of this group, for example, was the design of the Pixel Array Detector chips that are primary data acquisition instruments at SLAC’s Linac Coherent Light Source.

Instrument overview, capabilities, and resources

The F3 station is a versatile bend-magnet station that provides a variety of experimental capabilities. The radiation from the 5.3 GeV positrons, 21.6 m upstream from sample, has critical energy of 10.3 keV. The standard monochromator is double-crystal Si(111), tunable from 7 to 31 keV. A sagittal focusing second crystal is available, which focuses about 3 mrad of bending magnet radiation. White-beam and monochromatic mirrors may be used to provide a doubly-focused beam. Alternatively, multilayers with bandpass around 0.6%, 0.22%, 5% and 10% can be used, providing higher flux than Si-111 over an energy range of 5-20 keV. Si(220) crystals can also be used for better energy resolution. CHESS single-bounce mono-capillaries are used for microbeam focusing.

With capillaries focusing, scanning XRF microscope is approaching 10 micrometer spatial resolution. By expending X-ray beam in vertical direction with asymmetric Si(111) crystal, TXM and X-ray tomography has been implemented for large samples with field of view up to 9 mm by 9 mm. X-ray diffraction, X-ray protein crystallography with 0.22% energy bandwidth multilayers are also available. EXAFS and XANES have been implemented in transmission, fluorescence and grazing incident fluorescence mode at F3.

Various detectors and software packages are available for F3 experiments, such as scintillator coupled Andor camera, Quantum-4, Pilatus 200K and 300K, 4-element Vortex SSD and the recently available Maia 384 element detector. Praxes using PyMca libraries and GeoPixe are available for XRF data processing.

University of Puerto Rico – Rio Piedras (UPR-RP)

The UPR-RP, a predominantly Hispanic-Serving institution, is a state-funded, public, co-educational institution that was established in 1903 as Puerto Rico’s first institution of higher education. It is a multilevel system with three campuses, two university colleges, five regional colleges, and other specialized units throughout the island. The UPR system is generally recognized as the top-rated center for higher education in Puerto Rico. Only three UPR campuses offer graduate programs: Mayagüez, Medical Sciences, and Río Piedras. Of these, the UPR-Río Piedras is the oldest, largest, and most diverse one, featuring the most extensive research and library resources and supporting the broadest academic offering. Among all graduate programs, doctoral and master programs are offered in Chemistry at UPR-Río Piedras. UPR-RP has been accredited by the Middle States Association of Colleges and Universities since 1946, with corresponding accreditation per specialized school or program, and has been classified as a Doctorate Intensive Institution by the Carnegie Council. UPR-Río Piedras serves over 18,000 students (20% graduate) and grants an average of 3,000 (graduate and undergraduate) degrees per year. From 2009-2017 the Chemistry Graduate Program has been able to obtain $48M in external funds from different agencies.

Molecular Science Research Center (MSRC)

Laboratory (Figure 1): The MSRC is situated at one (1) mile from UPR-RP with a convenient 5 min public transportation connection (Urban Train), walking distance from UAGMC, and ca. 13 miles in a highway (<30 minutes commute) from UAGMG.

(A)

(B)

(C)

Figure 1. (A) The University of Puerto Rico’s Molecular Sciences Research Center (MSRC) provides the necessary environment, equipment and infrastructure to perform part of the proposed research activities; (B) many 12 ft. laboratory benches, and (C) 6 ft. laboratory fume hoods.

The MSRC, inaugurated in 2011, is an advanced state-of-the-art research facility designed for the country’s most competitive scientists. The Center provides an advanced infrastructure to conduct cutting-edge research, including molecular sciences, technology transfer, and commercialization. The MSRC houses 25 core faculty members from multiple disciplines across the UPR system, which provides a unique pool of expertise and fosters interdisciplinary collaborations among researchers as well as with federal agencies and the private sector ((bio)pharmaceutical industry), to solve common scientific challenges. Faculty members affiliated with the MSRC are funded through various mechanisms such as federal (NSF, NIH, NASA), and local agencies (Puerto Rico Science, Technology, and Research Trust). Currently, 290 researchers (20 postdocs, 120 graduate students, and 150 undergraduate students) perform research activities at the MSRC. Active research support from federal and local agencies exceeded $45 million since 2014.

Thus, the MSRC provides a robust and productive research and training environment for the research personnel (principal investigators, graduate and undergraduate students) involved in the proposed research activities. Dr. Jorge Colón, and Dr. Ratnakar Palai currently have assigned bench spaces (Figure 1B) at the MSRC. As Co-PIs of this NSF PREM Center, Dr. Mitk’El Santiago, Dr. Lymari Fuentes Claudio, Dr. Lisandro Cunci, and their personnel will also have access to multiple shared resources including major research instrumentation necessary to conduct the proposed activities and the technical assistance of expert scientists provided by each of the core facilities at the MSRC. The collaboration of the researchers and students at this state-of-the-art research facility will impact the retention of the students and will help them follow a pathway toward degree attainment.

Core Facilities at UPR’s MSRC: The multidisciplinary MSRC houses multiple state-of-the-art cores and facilities to meet the investigators needs for their individual research. The following most relevant facilities for the proposed research activities are available free of charge. The Materials Characterization Center (MCC) is located on the 1st floor of the MSRC. Four full-time technicians manage the shared major analytical equipment under good manufacturing practices, which are accredited by the FDA and many private companies from the (bio)pharmaceutical sector present on the island. The MCC provides access, training, and technical assistance for major research instrumentation in the area of Nuclear Magnetic Resonance (NMR), Mass Spectrometry, Surface Microscopy and Spectroscopy, and Confocal Imaging Microscopy. The MCC is directed by Dr. Edgard Resto (Department of Physics, UPR-Río Piedras) and Dr. José A. Prieto (Department of Chemistry, UPR-Río Piedras). The Crystallization Design Institute, directed by Dr. Stelzer, provides expertise-based molecular and engineering solutions for crystallization, materials characterization, solid form discovery and design, as well as crystallization and formulation process development. UPR’s Single Crystal X-ray diffraction facility (UPR’s SCXRDf) was recently inaugurated (2017). It provides easy access to crystallographic services (including micro powder X-ray diffraction) that are critical for solid-state materials’ characterization. The facility embraces a synergistic approach, providing training, instrument time, and technical support to users. The UPR’s SCXRDf was realized through a recent Major Research Instrumentation Grant from the NSF (CHEM-1626103) and is directed by Dr. Piñero from the Department of Chemistry, UPR-RP.

Major Equipment

Shared Laboratory Equipment available at UPR’s MSRC: The most relevant equipment necessary to carry out the proposed research activities is available at the MSRC as listed below.

• Polarized optical microscopes (Zeiss and Nikon)
• Raman spectroscopy microscope (ThermoScientific)
• Fourier transform infrared spectrophotometer (FTIR) microscope (ThermoScientific)
• Fourier transformed infrared spectrophotometer (Bruker)
• X-ray diffraction system (Rigaku SmartLab) for powder diffraction, thin-film diffraction, SAXS, in-plane scattering, high temperature and atmosphere control (pressure and gases) diffraction
• Single crystal micro focused X-ray diffractometer (Rigaku XtaLAB SuperNova) equipped with a HyPix3000 X-ray detector, a Cu-Kα (λ = 1.5417 Å) radiation source and an Oxford Cryosystems Cryostream 800 cooler for low and variable temperature measurements. The XtaLAB SuperNova is also able to work on micro-powder X-ray diffraction mode, which facilitates the examination of small quantities of samples
• Scanning Electron Microscope (SEM) equipped with Evenhart Thomley for secondary electron imaging (SEI), and a three-segment solid-state backscattered electron detector for Compo, Topo and Shadow Mode imaging (JEOL JSM-6480LV)
• High pressure liquid chromatography (Agilent 1100) with UV-vis diode array detector
• Laboratory scale hot melt extruder (ThermoScientific, MiniLabII)
• Rheometer (temperature-controlled, Anton Paar, MCR 302)
• Automated imaging system with incubator (Formulatrix, Rock Imager 54)

Researchers at the University of Puerto Rico

Dr. Ratnakar Palai’s laboratory spaces at the MSRC and UPR-RP are equipped with a variety of materials characterization instrumentation, which will be employed to carry out the proposed research activities. The most relevant equipment is listed below,

• RF plasma assisted molecular beam epitaxy (MBE) with six effusion cells
• Pulsed laser deposition (PLD) for growth of oxide/multiferroic thin films
• Atomic layer deposition (ALD)
• Sputtering
• Hall effect setup
• Current-voltage measurement system (10K-600K).

Dr. Ratnakar Palai has an Associate Professor appointment at the University of Puerto Rico – Rio Piedras. He has been highly active in the organizacion of annual and biennal conferences in Puerto Rico “Workshop on Multifunctional Nanomaterials” and “Workshop in Frontier in Electronics” since 2009. Dr. Palai has several continuous collaborations with other researchers including Dr. Julian Velev in the area of theoretical condensed matter physics.

Dr. Jorge Colón has a Professor appointment at the University of Puerto Rico – Rio Piedras,  has laboratory spaces at the MSRC and UPR-RP.  His research group has been highly active in the outreach in Solar Energy initially in collaboration with Caltech as part of the CCI-Solar Fuels Program. Dr. Colón has had collaborations with many researchers that includes a collaboration with Dr. Thomas Jaramillo at Stanford University to address catalytic properties of metal-incorporated nanoparticles, which is relevant to this proposal. Additionally, to his access to the MSRC, Dr. Colón has access to the facilities to Texas A&M that include the use of different instrumentation (e.g. Solid-state 31P NMR, XRPD, XPS, TGA, etc.) due to research collaborations.

Office: All PI and Co-PIs have fully furnished office spaces. Dr. Jorge Colón and Dr. Ratnakar Palai have office spaces located in the same building as their laboratories at UPR-RP. Dr. Mitk’El Santiago and Dr. Lymari Fuentes Claudio have office spaces at Universidad Ana G. Méndez. Dr. Lisandro Cunci has office space at Universidad del Turabo. Each office space provides Internet, phone, and printing support and convenient access to fax, copy, and shared full-time staff assistants within the MSRC, UPR-RP, UAGMC, and UAGMG.

Computer: The combined laboratory spaces are equipped with laptop and desktop computers; all are password, firewall, and virus protected. All computers have Internet access and are configured with standard application software for Windows systems, including Microsoft Office 365, Acrobat (Adobe Systems, Inc.), Mercury (Cambridge Structural Database, CSD), and ChemDraw (PerkinElmer). The computers are integrated into the password protected MSRC local area network, which provides high-speed Internet and network connections.

UPR-Río Piedras online libraries, SciFinder Scholar, Scopus, MEDLINE, numerous on-line journals, webCSD, and a variety of other databases.

Other resources

Additional Equipment at MSRC: The MSRC is a highly collaborative environment, should the proposed research activities lead in a direction where additional equipment is required core faculty members of the MSRC have an unrestricted access to the following additional equipment,

• 300 MHz NMR (Bruker), Ascend Aeon 500 MHz NMR (Bruker), and 700 MHz NMR (Bruker). A H-C-N probe for solid-state NMR capabilities will be acquired for the 700 MHz NMR system within the next few months.
• VG-Fisons Autospec High Resolution MS System with GC / MC, DIP, FAB, LSIMS, EI and CI modes,
• VG-Fisions Quatro MS / MS system with GC / MS, HPLC / MS, Ei and CI modes, APCI and direct sample introduction options
• Hewlett Packard 5995A with GC/MS (capillary and package columns), DIP, thermal and packed columns), DIP thermal desorption sample introduction
• Hewlett Packard MSD GC/MS system
• Digital Instrument Nanoscope IIIA Atomic Force (AFM) and Scanning Tunneling (STM) Microscopes
• Biospectrum 810 UVP, Visible and UV Imager (2)
• EC3 BioChemi Imaging System
• Biotek Synergy H1 Microplate Reader
• Guava Easy-Cyte Flow Cytometry (Millipore).
• High Speed and Ultra High Speed Centrifuges (2)
• Tecan Infinite M200 PRO Microplate Reader
• Micropipette Puller Sutter Instrument
• Ultimaker 3, 3D Printer
• Zeiss Primo Vert Inverted Microscopes
• Eppendorf Microcentrifuges
• Refrigerated Eppendorf Microcentrifuge
• Genesys 10S BioUV Spectrophotometer w/ thermal printer
• Leica Cryostats
• Vacufuge w/pump
• VWR -20 °C Upright Freezers
• THERMO -80 °C Ultra Low Freezers
• FISHER CO2 Incubators
• AGILENT G4900DA Surescan Microarray Scanner
• Lab Conco Port Drying Chamber w/Pump
• Milli Q-16 Water Purification System—Free of DNA’ases
• Nikon Digital Microscopes
• Buchi 210 Rotoevaporators
• Analytical Balances
• pH meters
• Hot plate stirrers

Additional Equipment at UPR-RP:

• Nanoscopy Facility: Ultrahigh Resolution Field Emission 200kV STEM/TEM with Cs Probe Corrector (i.e. STEM Corrector), Omega Energy Filter, and large area X-ray detector; Conventional 200kV STEM/TEM LaB6 with XRF and Omega Filter; Focused ion beam (FIB) microscope; optical microscope with micromanipulators; High Resolution Field Emission Scanning Electron Microscope with X-ray fluorescence detection and STEM holder.

Universidad Ana G. Méndez, Cupey Campus (UAGMC)

Universidad Ana G. Méndez  (UAGM) has the physical and human resources required to perform the proposed project. Dr. Lymari Fuentes Claudio has 150 sq ft of laboratory space, located in the main campus at UAGM. In addition, a tissue culture room (300 square feet) and a microscope room are available. Equipment is located throughout the first and third floor of the IC building (2,400 square feet). Facilities for ultrapure water (Millipore), as well as an autoclave room are available in the Muñiz Souffront building, next to the IC building.

Office. The Co-PI office space is 70 square feet and have a computer with Internet access; it is located at the Division of Sciences and Technology Building.

Major Equipment. Major equipment available to support research includes: Rigaku Miniflex X-ray diffractometer, Shimadzu UV-vis NIR 3600 spectrophotometer with capacity to perform solid state diffuse reflectance spectroscopy, Gamry potentiostat/galvanostat with capacity to Impedance spectroscopy, 1 StepOne (Applied Biosystem), 2 Nanodrops, 2 Countess™ Automated Cell Counters (Invitrogen), 1 enzyme-freezer, 4 environmental shakers, 3 Labline incubators, 3 laminar flow hoods, Bio-Rad electrophoresis documentation system, Bio-Rad agrasose and protein gel electrophoresis, Marathon refrigerated centrifuge, Eppendorf microcentrifuges, 2 Millipore water distiller/deionizer, Stuvall hybridization water bath, Labline hybridization oven, Bio-Rad gel dryer, Olympus fluorescent microscope with digital camera, Nikon inverted microscope, Waters HPLC with florescence detector, Waters GC with flame ionization and thermal conductivity detectors, Waters MS, Varian UV-vis Spectrophotometer, Promega GeneQuant RNA/DNA calculator, Varian SpectrAA atomic absorption, Varian 3800 GC with flame ionization and thermal conductivity detectors, Dionex ion chromatographer, 4 thermal cyclers, 1 Thermo-forma CO2 incubator, Savant Speedvac, UV cross-linker, 2 water distillers/deionizers, ice machine, 3 large capacity laboratory refrigerators, 3 small capacity laboratory refrigerators, 2 large capacity laboratory freezers, Varian Eclipse Spectrofluorimeter.

Library. The library is located very close to the laboratory and has internet access to multiple databases in the areas of science and health.

Universidad Ana G. Méndez, Gurabo Campus (UAGMG)

Students participating in this NSF PREM Center will have complete access to the facilities and training at UAGMG; as well as the facilities at the Puerto Rico Energy Center (PREC), a materials characterization center funded in part by the Department of Energy (DoE), and the facilities located at the laboratory of Dr. Lisandro Cunci and collaborators. In each of the facilities that the students will have access, there are experts dedicated to train students, postdocs and professors in the use and theory of each instrument.

Dr. Lisandro Cunci has an Associate Professor appointment at Gurabo Campus, currently with 75% of release time. As a new professor, his research group has just started developing outreach programs recently. Dr. Cunci currently has collaborations with researchers in different institutions that include Dr. Jessica Koehne at NASA Ames, Dr. Carlos Jimenez at the University of Puerto Rico, and Dr. Jorge Almodovar at Gurabo Campus, among others. Additionally, to his access to the MSRC, Dr. Cunci has access to the Puerto Rico Energy Center which has many research instrumentations which are detailed in the following paragraphs.

Laboratory and Facilities at School of Natural Sciences and Technology and Puerto Rico Energy Center, UAGMG:

Universidad Ana G. Méndez, Gurabo Campus is equipped with laboratory facilities that include approximately 23,500 sq. ft. of laboratory, preparation, storage, and waste disposal space in the science laboratory building. The following scientific instrumentation related to this project is available at Dr. Lisandro Cunci’s laboratory:

– Two (2) Gamry Reference 600+ Potentiostats with computer

– Bio-Logic SP-200 Potentiostat with computer

– Waveneuro Potentiostat from PINE Research with PCIe-6363 NI board with computer

– Multimode Microplate reader Tecan M200PRO

– Nikon FN1 Fixed Stage Upright Microscope with DIC and long WD objectives

– Epi-fluorescence in the Nikon FN1 Microscope with LED excitation X-Cite XLED1

– 3-axis Water Hydraulic micromanipulator MHW-3

– Micropipette puller Narishige

– Biosafety Cabinet Type II/A

– Two (2) CO2 incubators

– Inverted microscope

– Flow cell system with computer-controlled syringe pump

– Mini-CNC for electronic circuit fabrication

– 3D Printers Prusa I3 and da Vinci mini

– High Capacity Freeze Drying System LABCONCO

– 4°C, -20°C, and -80°C Freezers connected to the Building’s Emergency Power Plant

– Eppendorf 5407, 5424, and 5430 high speed microcentrifuges

– pH Meter Mettler-Toledo

– Analytical Balance Mettler-Toledo

– Dionex-1500 Ion Chromatography with autosampler

Dr. Lisandro Cunci also has access to the following instrumentation at UAGMG in the School of Engineering and Puerto Rico Energy Center:

Atomic Absorption (AA) Spectrometer with Graphite Furnace, Autosorb 1-MP and iSorb HP-1 adsorption analyzers, Fourier Transform Infrared (FT-IR) Spectrometer, Gas Chromatograph (GC), Gas Chromatograph- Mass Spectrometer (GC-MS), Water purification system, CARVER Hydraulic Press, Total Organic Carbon (TOC) Analyzer, UV-2401 Spectrophotometer, Biologic Modular Potentiostat, Genetic Analyzer, Tube Furnace, Helix Supercritical Dryer, High Performance Liquid Chromatograph (HPLC), Thermogravimetric Analyzer, UV-Vis 1800 Spectrophotometer, Fluorescence Spectrophotometer, X-Ray D8 Advanced, NMR Spectrometer Bruker Aeon 400 MHz liquid/solid, Scanning Electron Microscope (SEM/EDS) JEOL JSM-6010LA, Xevo Ultra Performance Liquid Chromatography (UPLC), two (2) Ultra low temperature Freezers -80 °C, and two (2) Low temperature Freezers -20 °C.