Structural Analysis
Nuclear Magnetic Resonance (NMR)
The NMR Laboratory at ARC offers advanced nuclear magnetic resonance (NMR) spectroscopy tools for studying small molecules, macromolecules, and complex materials. Our lab supports a wide range of research in chemistry, biochemistry, materials science, and related disciplines, with both self-use and full-service options available, both to CSU and external users.
Services:
- Liquid-state NMR for small molecules, natural products, and macromolecules.
- Solid-state NMR (coming soon): for studying insoluble materials, soil, polymers and crystalline solids.
- Structural elucidation of small molecules and reaction products.
- Quantitative NMR (qNMR) for accurate concentration and purity determination.
- Variable-temperature (VT) experiments for temperature-dependent studies.
- Method development for non-routine or low-abundance nuclei.
- Expert consulting on experimental design and data interpretation.
Instruments:
- Agilent (Varian) 400MR: 400 MHz NMR for liquid samples, equipped with Automated Tuning and a 7600 Sample Changer.
- Bruker US400: 400 MHz NMR for liquid samples, equipped with BBFO SMART ProbeTM and 24 sample SampleCaseTM.
- Bruker NEO400: 400 MHz NMR for liquid samples, equipped with a ProdigyTM BBFO Probe and 24 sample SampleCaseTM.
- Bruker Ascend 400: 400 MHz NMR for liquid samples, equipped with BBFO smart probe, and extended range VT.
Coming Soon:
- Bruker AVANCE NEO 600 MHz NMR with solid-state capabilities (funded by NSF-MRI).
- Bruker AVANCE NEO 400 MHz NMR with 60 sample SampleCaseTM (funded by NIH-SIG S10)
Contact: Dr. Michele Mailhot
Mass Spectrometry
The Self Use Mass Spectrometry (MS) Laboratory at ARC provides a diverse range of mass spectrometry solutions for molecular identification, structural analysis, and quantitative applications across various sample types. Our instrumentation supports gas chromatography (GC), liquid chromatography (LC), infusion, dried, and thermal desorption techniques, offering flexibility for a wide range of analytical needs.
Services:
- Molecular Identification & Structure Determination – Accurate mass analysis for molecular formula confirmation and fragmentation pattern analysis.
- Intact Protein Analysis – Molecular weight confirmation and detection of post-translational modifications.
- Polymer Characterization – MALDI-TOF/TOF analysis for molecular weight determination (0.5–500 kDa) and end-group analysis.
- Targeted & Untargeted Analysis – Precise screening and quantification of specific analytes and data-driven profiling of complex mixtures.
Instruments:
- Agilent 6545 Q-TOF LC/MS (“TOF-U”) – Used for accurate mass analysis, metabolomics, and lipidomics. Features high resolution (45,000 FWHM) and mass accuracy (<1 ppm).
- Thermo ISQ with Markes Thermal Desorption GC/MS – Ideal for structure confirmation and quantitation of volatile compounds with thermal desorption. Comes with offline Markes TD tube desorption system.
- Thermo TSQ GC/MS – Targets quantitative assays for volatile compounds with triple quadrupole mass analysis.
- Bruker UltrafleXtreme MALDI-TOF/TOF – High-resolution MALDI-TOF/TOF mass spectrometer for analyzing macromolecules and small molecules, offering femtomolar sensitivity and advanced structural analysis.
Contact: Dr. Claudia Boot
Spectroscopy
Our Spectroscopy Laboratory provides a range of analytical tools for the characterization of molecular structure, composition, and interactions across various sample types.
Services:
- Molecular Characterization – Analyze molecular vibrations, functional groups, and chemical bonding in solids, liquids, and gases for a wide range of sample types.
- Fluorescence Analysis – Characterize fluorescent molecules, quantify molecular interactions, and study electronic transitions in materials and biological systems.
- Particle and Nanomaterial Analysis – Measure particle size, distribution, and stability in colloidal suspensions, nanoparticles, and macromolecules in solution.
Instruments:
- Edinburgh FS5 Spectrofluorometer – High-performance fluorescence spectrometer with a 150 W xenon lamp for excitation (200-1000 nm) and emission detection (230-870 nm). Features fluorescence lifetime measurements (TCSPC), temperature-controlled and solid sample holders, and an integrating sphere for quantum yield measurements.
- Malvern Zetasizer Nano ZS – Uses a 633 nm red laser for particle size analysis (DLS), zeta potential measurement for colloidal stability, and microrheology of protein and polymer solutions. Also enables molecular weight determination of macromolecules.
- Nicolet iS-50 FT-IR Spectrometer – Equipped with multiple sampling accessories:
- ATR-Diamond or Germanium crystal for thin films, powders, and liquids.
- Harrick Grazing Angle Reflectance for thin films on metal or semiconductor substrates.
- Gemini Diffuse Reflectance for non-reflecting powder materials.
- Transmission Mode sample holder and KBr pellet press for preparing transmission experiments.
- Perkin Elmer Frontier FTIR with Spotlight 400 microscope – automated micro FTIR analysis:
- Reflectance, transmission, and Ge-ATR with ~6.5 μm resolution
- Operates in point mode and a scanning mode for automated sampling
- Automated sample stage for large area (2 mm x 2 mm) optical and IR mapping
- Equipped with a high sensitivity Cadmium Mercury Telluride (CMT) detector
- Gold coated filters and filtering apparatus available on request for microplastic analysis
Contact: Dr. Indrani Bhowmick for fluorometer and DLS | Dr. Ethan Crace for FTIR instruments
X-ray diffraction & crystallography
The X-ray Diffraction (XRD) and Crystallography Laboratory at ARC provides structural characterization for a wide range of materials, with a specialized focus on small-molecule and hybrid organic-inorganic material single-crystal X-ray diffraction (SCXRD). Our team offers expert support across the full workflow, from crystal growth and screening to unit cell determination, structure solution, refinement, and CIF preparation for publication.
We are particularly experienced in solving complex structural issues, including twinning, disorder, and absolute structure determination. We routinely support high-quality, publication-ready results. Our facility also offers automated crystallization screening using a robotic platform to improve crystal growth success rates through batch optimization at the microliter scale.
The lab operates in both full-service and self-use modes, with guidance available for experimental design, crystallization strategies, and structural analysis via staff office hours and additional times on request.
Services:
- X-ray Diffraction for Powders – Determine structural properties, phase composition, and approximate crystallite size. Air-sensitive sample holders available for analysis of sensitive samples. Variable temperature analysis available on request (see below). Sample amounts as low as ~50 mg can be analyzed with zero background holders.
- Single-Crystal X-ray Diffraction – Obtain high-resolution 3D molecular and crystal structures for small-molecule, hybrid materials, and inorganic compounds, including complex or disordered systems. System accommodates air sensitive samples and can perform variable temperature analysis. Crystal sizes of approximately 50-100 micrometers are typically successful.
- Crystallization Support and Screening – Expert assistance with crystal growth using a range of methods (e.g., vapor diffusion, evaporation, layering, and solvothermal methods), including automated high-throughput screening for optimal crystallization conditions for isothermal crystallization techniques.
- DEA licensed for Schedule II-IV Samples: Our Core Facility is authorized under a DEA license to receive, handle, and analyze controlled substances classified as Schedule II–IV. This includes active pharmaceutical ingredients (APIs) and other regulated compounds.
- Single-crystal XRD for structure determination and absolute structural confirmation
- Powder XRD for phase identification and polymorph analysis
Instruments:
- Bruker D8 Discover DaVinci (Powder XRD) – Non-destructive phase analysis including approximate particle size, of polycrystalline and thin film samples in reflectance or transmission mode. Air-free and zero-background (Si or SiO2) sample holders available on request. Default sample stage is the FLIPSTICK 9-slot sample changer for automated sample analysis. System has divergent beam optics only. Detector is a Lynxeye XE-T detector with energy discriminator to filter Cu Kβ and x-ray fluorescence. System has an optional Anton Paar HTK-1200N stage for variable temperature capabilities (25–1200 K) under air or vacuum. Variable temperature samples can be placed in capillaries or a corundum (Al2O3) sample stage.
- Bruker D8 Advance QUEST (Single Crystal XRD) – Determines crystal structures of small-molecule, hybrid, and inorganic single crystals. System is equipped with a Mo Kα x-ray source, Photon 50™ detector, and Oxford cryostat for variable temperature control (80–400 K) and air-free sample handling. System can also accommodate powder samples in capillaries for variable temperature powder measurements.
- Crystallization Robot – Supports automated batch crystallization and screening of diverse conditions for small-molecule compounds, optimizing crystal growth for Single Crystal XRD. Restrictions on highly volatile and toxic solvents and reactive or acutely toxic samples at staff’s discretion.
Contact: Dr. Ethan Crace
