msu_chemistry service center

Chemistry Service Center

Chemistry Service CenterServices & Capabilities

Mission Statement: To support collaborative research at Mississippi State University and to build partnerships with both the public and private sector by providing access to advanced instrumentation and technical knowledge


Tonia LaneManager, Chemistry Service Center

M.S. Biochemistry, UT Knoxville

SmithKline Beecham, King of Prussia, PA • Assay Development in Drug Discovery

IGEN (BioVeris), Gaithersburg, MD• Assay development & validation in

Contract Services ISO, GLP

New Mexico State University, Las Cruces

NM• Lab Manager• HHMI-NMSU Programs

Sapphire Energy, Las Cruces NM• Group Leader, Field Analytical

Lab

Mississippi State University • Manager, Chemistry Service

Center


INSTRUMENTATION


Nuclear Magnetic Resonance Spectroscopy (NMR)

• Bruker Avance III 300 MHz: Routine 1D 1H NMR spectra (typically of small molecules).

• Bruker Avance III 500 MHz: Longer NMR experiments such as 13C, 195Pt and other NMR active nuclei; as well as variable temperature NMR experiments.

• Bruker Avance III 600 MHz: High quality 1D NMR spectra; and complex 2D NMR experiments like COSY, NOESY, HSQC, and HMBC on both small molecules and proteins.


X-Ray Crystallography (XRD)

Capabilities:• Unambiguous identification of molecular structure of small molecules • Protein crystal evaluation prior to sending to a synchrotron for

solution

Features:• In-line, high brilliance, dual Micro-sources:

– Molybdenum source for routine high throughput small molecule samples

– Copper source for specialized experiments designed to obtain information about absolute stereochemistry.

• CMOS camera technology for rapid data collection• Software for rapid solution of data sets

Air-cooled Bruker D8 Venture XRD with IμS microfocus source


High Resolution Mass Spectroscopy

Bruker UHPLC micOTOF-QII high resolution mass spectrometer for high quality mass analysis.

Reverse phase ultra-high performance liquid chromatography (UHPLC) on complex liquid mixtures.

Direct injection of purified liquids and solids (both small molecules and larger biomolecules). 3 ionization source attachments:• electrospray ionization (ESI) – high voltage, standard ionization

method• atmospheric pressure photoionization (APPI) – UV light,• atmospheric pressure chemical ionization (APCI) – corona discharge

needle


Atomic Absorption Spectroscopy (AAS)

Samples are atomized by a flame atomizer that can be set to acetylene-air (about 2300°C) or acetylene-nitrous oxide (about 3000°C).

Analysis of any given element on the AAS requires a hollow cathode lamp specific for that element, as each element absorbs unique wavelengths of light.

Available lamps: Ag, As, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Ni, P, Pb, Rh and Zn.

Additional lamps can be purchased if necessary.

The Shimadzu AA-7000 atomic absorption spectrophotometer is used to determine concentrations of elements in homogeneous solutions.


Fourier Transform Infrared Spectroscopy (FT-IR)

The Thermoscientific Nicolet 6700 FT-IR is equipped with two modes of data collection:

• attenuated total reflectance (ATR): analysis of pure solids, pure liquids or solution samples

• diffuse reflectance (DRIFT): analysis of fine powder samples

Data is collected as an absorbance or transmission spectrum. The spectral range of the instrument is 400 – 4000 wavenumbers (cm-1). Samples must be air stable.


Electron Paramagnetic Resonance(EPR)

The Bruker EMX-10 EPR collects routine spectra of organic and inorganic radicals from room temperature to liquid nitrogen temperatures (~77 K).


Gas Chromatography – Mass Spectroscopy (GC – MS)

The Shimadzu QP-2010S GC-MS separates liquid mixtures based on polarity followed by component analysis via mass spectrometry. • components are separated in the GC producing a total ion count (TIC)

chromatogram • the individual peaks in the chromatograph corresponds to individual

compounds• Each peak can be analyzed by mass spectroscopy

Currently:• electron ionization (EI)• nonpolar column, temperature range from

ambient to 300°C• manual injection of about 1 to 2 µL


High Pressure Liquid Chromatography – Mass Spectroscopy (HPLC-MS)

The Agilent 1200 series HPLC-MS separates complex liquid mixtures into individual components and analyzes each component via mass spectrometry.

• UV detector can monitor a single wavelength in the range of 190 to 600 nm

• UV readout and a total ion count (TIC) chromatogram. The instrument can provide a mass spectrum for each of the peaks • Set up to do reverse phase chromatography• The MS has an atmospheric pressure ionization

electrospray (API-ES) source & a mass range of 10 – 1500 m/z

• Currently, we have no databases for compound identification based on their mass spectrum.


Differential Scanning Calorimetry (DSC) Measures the difference in the amount of heat required to increase the temperature of a sample and reference to the same degree. • Data is usually presented as a heat flow versus temperature graph. • Temperature range: ambient to 725°C. • Available sample pans (both can be heated to temperatures up to

600ᵒC) : – aluminum – alodined aluminum (for aluminum reactive materials)

The TA Instruments Q20 DSC data can be used to determine thermodynamic values such as:• glass transition temperature (Tg), • melting temperature (Tm)• crystallization temperature (Tc)• enthalpies of phase changes• heat capacities


Thermogravimetric Analysis (TGA) The TA Instruments Q50 TGA measures the properties of a material based on increasing temperature over time. During the heating process materials can undergo % gain or loss due to oxidation, decomposition or some other process and many materials have distinct decomposition patterns.

• Data is presented as a % weight verses temperature graph.

• Samples can be heated under inert (nitrogen) or atmospheric (air) conditions.

• Temperature range: ambient to 1000°C.

• Platinum sample pans to minimize reactivity between the sample and the pan.

• Sample loadings are typically a few milligrams.


UV-Vis Spectroscopy

Shimadzu UV-2550 UV-Vis spectrophotometer:

• measures absorbed at wavelengths of 190 – 900 nm.

• temperature control from ambient to 60°C.

• available cuvettes:

– quartz (range: 170 to 2700 nm)

– methacrylate cuvettes (range: 285 to 800 nm)


MSU Customers External CustomersInstrument Self-Use Assisted Use Non-profit Commercial

NMR-600 MHz $12 / hour $62 / hour $90 / hour $135 / hour

NMR - 500 MHz Contact for pricing Contact for pricing Contact for pricing $135 / hour

NMR-300 MHz $8 / hour $58 / hour $85 / hour $135 / hour

Single Crystal XRD $275 / solution $325 / solution $470 / solution Contact for pricing

High Res MS (direct inj) $15 / hour $15 / sample $50 / sample $180 / sample

High Res MS (UHPLC) $50 / hour $50 / sample $100 / sample Contact for pricing

AAS (Curie Lab) $ 5 / hour $5 / sample $20 / sample Contact for pricing

FT-IR (Curie Lab) $5 / hour $5 / sample $20 / sample Contact for pricing

LC-MS (Curie Lab) $20 / hour $30 / sample $60 / sample Contact for pricing

GC-MS (Curie Lab) $15 / hour $15 / sample $30 / sample Contact for pricing

GC-FID $5 / hour $5 / sample $20 / sample Contact for pricing

TGA/DSC (Curie Lab) $5 / hour $5 / sample $20 / sample Contact for pricing

ICP-MS (plus standards) $50 / hour $50 / sample $100 / sample Contact for pricing

UV-Vis (Curie Lab) $5 / hour $5 / sample $20 / sample Contact for pricing

Instrumentation training fee: $50/hour Prices are subject to change. Contact us for the current pricing schedule.


OPERATIONAL STAFF


Xue “Snow” XuClinical Assistant Professor

Snow Xu is currently involved with chemical education and NMR spectroscopy management. She previously used NMR spectroscopy to study organic small molecules as part of her research on using metalloradical catalysts to develop stereoselective chemical processes for the construction of multifunctionalized organic molecules. Her research effort has led to several high impact journal articles, including six published in J. Am. Chem. Soc. and two in Angew. Chem. Int. Ed.. Due to the significance and depth of her research, she was nominated as one of the 45 finalists of the 2013 Reaxys Ph.D prize. Dr. Snow Xu earned her Ph.D. in Organic Chemistry from University of South Florida with Dr. Peter Zhang (currently in Boston College).


Sean StokesInstrument Manager

Sean Stokes handles the day-to-day maintenance and operation of service center instrumentation. He is an organic chemist with over 8 years’ of experience running and interpreting NMR, HRMS, HPLC, GC and FT-IR. Dr. Stokes holds bachelor’s and master’s degrees from the University of Alabama in Huntsville and a doctorate in chemistry from Mississippi State University.


N. Radhika ReddyNMR Manager

N. Radhika Reddy ensures that the NMR facility is operating effectively. She also handles student and staff training and sample analysis for external users. Dr. Reddy is a synthetic organic chemist with over 7 years’ experience with NMR and IR; and with over 5 years’ experience with GC and mass spectroscopy. She holds a master’s degree from Tennessee Tech University and a doctorate in chemistry from Mississippi State University.


Henry ValleGraduate Assistant, X-ray Crystallography

Henry Valle is currently a graduate student in the Department of Chemistry and uses x-ray crystallography in his organometallics research. Henry maintains and operates the Bruker D8 Venture XRD. He is working on his doctorate in chemistry at Mississippi State University and holds a master’s from California State University, Los Angeles.


FACULTY ADVISORY GROUP


Alan I. MarcusWilliam L. Giles Distinguished Professor and

Interim Head, Department of Chemistry

As the Interim Head for the Department of Chemistry Alan Marcus oversees Chemistry Service Center activities. A historian of chemistry and of institutions, Marcus has written on the development of management strategies, establishment of state and federal regulation and regulatory agencies, creation of U. S. science policy since 1950 and the formation of the modern agricultural research establishment. Dr. Marcus holds a bachelor’s degree from the University of Wisconsin-Madison and a master’s and doctorate from the University of Cincinnati.


Keith HollisAssociate Professor,

Department of Chemistry

Keith Hollis is an organometallic chemist whose lab utilizes x-ray crystallography to develop novel CCC-NHC organometallic pincer complexes. Dr. Hollis has authored 48 peer-reviewed publications and has active collaborations with chemists from around the Dr. Hollis holds a bachelor’s degree in Chemistry from Huntingdon College, a doctorate degree in Inorganic Chemistry from the University of Chicago and a doctorate degree in Organic Synthesis from the University of California, Irvine.


Nicholas FitzkeeAssistant Professor,

Department of Chemistry

Nicholas Fitzkee is broadly interested in using NMR spectroscopy to study the molecular basis of protein adsorption to surfaces. His group works to develop novel, NMR-based techniques for understanding protein-surface interactions. A major goal of his research is the development of customized, protein-based nanoconjugates for biomedical diagnostics and therapeutics. Such systems could be used as highly selective molecular sensors or effective drug delivery tools. Dr. Fitzkee earned his Ph.D. in Biophysics from Johns Hopkins University with Dr. George Rose, and he completed a postdoc at the National Institutes of Health with Dr. Ad Bax.


Contact Us

Department of ChemistryMississippi State University 1115 Hand Lab310 President’s CirclePhone: 662-625-7023Fax: 662-325-1618Email: [email protected]: www.chemistry.misstate.edu

mailto:[email protected]

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