Research Instrumentation/NMR Facility

Research Instrumentation Facility
Research Instrumentation Facility

Available Instruments

The Research Instrumentation Facility (RIF) is equipped with a wide variety of instrumentation for chemical analysis including NMR, optical spectroscopy, thermal analysis and GC-MS.

NMR

Bruker Avance III-HD 700 MHz
Bruker Avance 600 MHz NMR
Bruker Avance III-HD 400 MHz NMR
Bruker Avance III-HD 300 MHz NMR
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Optical Spectroscopy

Shimadzu UV-2401 UV-VIS
Jasco 815 Circular Dichroism (CD)
Shimadzu RF-5301PC Fluorimeter
Rudolph Autopol III

Infrared Spectroscopy (FT-IR)

Smiths Detection SensIR IR Microscope
Nicolet AVATAR 380 FT-IR
Leica Optical Microscope
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GC-MS

Thermo Scientific Trace GC/Polaris Q MS
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Thermal Analysis

Perkin Elmer STA6000
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Other Instruments

Carl Zeiss Scanning Electron Microscope with Xray Detection System
Data Processing and Workstation Facility
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RIF Links
Research Uses
User Guides
Experiments

RIF Links

NMR Educational Sites

Research Uses

Nicolet380

  • Lee, J., Bartlet-Hunt, S., Li, Y., Morton, M. “Effect of 17β-estradiol on stability and mobility of TiO2 rutile nanoparticles”, Science of The Total Environment (Impact Factor: 3.16). 04/2015; 511. DOI: 10.1016/j.scitotenv.2014.12.054.

Solid State NMR

  • Vo, T. H., Shekhirev, M., Kunkel, D. A., Morton, M. D., Berglund, E., Kong, L., Wilson, P. M., Dowben, P. A., Enders, A., Sinitskii, A. “Large-scale solution synthesis of narrow graphene nanoribbons”, Nature Communications, 2014, 5:3189. DOI: 10.1038/ncomms4189.

Experiments

General Information

Sensitivity

  • Higher field gives better Signal-to-Noise and better signal dispersion, so 700>600>500>400>300 MHz. Linewidths in Hz are similar whatever the field, so the linewidths in ppm are smaller at the higher field strengths, unless a frequency-dependent line broadening mechanism interferes.
  • Probes optimized for a particular nucleus give the best signal to noise ratio (S:N) for that nucleus. The cryoprobes on the 700 MHz are indirect detection probes with the 1H electronics cooled to reduce thermal noise, and is thus most sensitive to proton. 
  • The 300 and 400 MHz have BBO-F probes with automatic tune and match (ATM). A wide range of nuclei are available on these probes. The give better resolution than prior probes due to the ATM and better receivers.

Proton Homonuclear

  • Availability:  H1 experiments are available on all instruments.
  • 1D Proton Experiment 
    • Default Parameters 
      • ~3 second acquisition time
      • ~2 second relaxation delay
      • Spectral width -4ppm to 16ppm
      • 16 scans
      • Total time: 2 minutes
    • Recommended concentration:  0.1 mM
  • Variations on the 1D experiment include: 
    • 1D NOE
    • 1D Selective COSY (gradient) though the 2D only takes 4 minutes
    • T1 determination
  • 2D COSY - Proton-proton correlation experiment 
    • Gives information about pairs of protons that are J-coupled. This usually indicates that the protons are on adjacent carbons, e.g., 3-bonds away (though protons further apart may in some cases be J-coupled).
    • Default Parameters 
      • 2 second relaxation delay
      • 1024 complex points in t2 and 128 increments in t1
      • 1 scan per increment
      • Total time: 4 minutes (cosygpsw)
      • Recommended Concentration:  1 mM
    • Variations on COSY 
      • DQF-COSY 
        • phase-sensitive experiment
        • diagonal peaks are narrower
        • less sensitive
      • TOCSY - total correlation spectroscopy 
        • gives correlations for all protons within a spin system
      • NOESY - Proton-proton through-space interactions via NOE 
        • Gives information about pairs of protons that are close in space (<5 A apart)
        • Default Parameters 
          • 1.5 second relaxation delay
          • 1024 complex points in t2 and 256 increments in t1
          • 2-8 scans per increment
          • Total time: 1 - 5 hours
          • Recommended Concentration:  at least 10 mM
      • ROESY - rotating frame NOE 
        • Compounds of molecular weight ~1000-2000
        • Exchange peaks are opposite sign from NOE peaks
      • HMQC - Heteronuclear Multiple Quantum Correlation experiment with DEPT editing
        • Gives information about strong proton-carbon J-couplings. A strong proton-carbon J-coupling indicates that the proton is directly bonded to the carbon. This experiment gives information that is identical to HETCORs or HMQCs, which are less sensitive. Additionally, it gives DEPT editing (color encodes – CH and CH3 versus CH2).
        • Default Parameters 
          • 1.5 second relaxation delay
          • 1024 complex points in t2 and 128 increments in t1
          • 4 scans per increment (hsqcetedgp)
          • Total time: 15 minutes
          • Recommended Concentration:  at least 10 mM
      • HMBC - Heteronuclear Multiple Bond Correlation experiment 
        • Gives information about weak proton-carbon J-couplings. A weak proton-carbon J-coupling indicates that the proton is two, three, or four bonds away from the carbon. This experiment gives information about which protons are near to (but not directly bonded to) different carbons. This experiment (in conjunction with the HSQC) can give an enormous amount of information about molecular structure, since the long range proton-carbon correlations can include quaternary carbons, in addition to protonated carbons.
        • Default Parameters 
          • 1.5 second relaxation delay
          • 1024 complex points in t2 and 128 increments in t1
          • 4 scans per increment
          • Total time: 25 minutes
          • Recommended Concentration:  at least 20 mM

Carbon Heteronuclear

  • H"M"QC - (Change to HSQC) -Heteronuclear "Multiple Quantum" (Change to "Single Quantum") Correlation experiment with DEPT editing
    • Gives information about strong proton-carbon J-couplings. A strong proton-carbon J-coupling indicates that the proton is directly bonded to the carbon. This experiment gives information that is identical to HETCORs or HMQCs, which are less sensitive. Additionally, it gives DEPT editing (color encodes – CH and CH3 versus CH2).
    • Default Parameters
      • 1.5 second relaxation delay
      • 1024 complex points in t2 and 128 increments in t1
      • 4 scans per increment (hsqcetedgp)
      • Total time: 15 minutes
      • Recommended Concentration: at least 10 mM
  • HMBC - Heteronuclear Multiple Bond Correlation experiment
    • Gives information about weak proton-carbon J-couplings. A weak proton-carbon J-coupling indicates that the proton is two, three, or four bonds away from the carbon. This experiment gives information about which protons are near to (but not directly bonded to) different carbons. This experiment (in conjunction with the HSQC) can give an enormous amount of information about molecular structure, since the long range proton-carbon correlations can include quaternary carbons, in addition to protonated carbons.
    • Default Parameters
      • 1.5 second relaxation delay
      • 1024 complex points in t2 and 128 increments in t1
      • 4 scans per increment
      • Total time: 25 minutes
      • Recommended Concentration: at least 20 mM

Phosphorus

  • The BBO-F probes will need to be tuned to 31P before acquisition with atma. The 600 BBO probe must physically be tuned to 31P. Sensitivity is approximately 15 times less than for proton, so adequate Signal-to-Noise for a reasonable length experiment (10 minutes, 256 scans) requires a concentration of > 0.1mM.
  • 1D Phosphorus experiment 
    • Default Parameters 
      • 0.8 second acquisition time with proton decoupling
      • 3.0 second relaxation delay (d1; with NOE enhancement)
      • Spectral width -100ppm to 250ppm
      • 32 scans
      • Total time: ~2 minutes
      • Recommended Concentration:  0.1 mM

NFluorine

The 400 and 300 MHz BBO-F probe is well-suited for direct observe 19F experiments. Tuning these probes to 19F uses the atma command. The 600 MHz NMR with the H/F probe gives the best sensitivity for 19F.

  • Sensitivity is approximately the same as for proton, so adequate S/N can be obtained with concentration > 0.1mM.
  • 1D Fluorine experiment 
    • Default Parameters 
      • 0.8 second acquisition time
      • 3.0 second relaxation delay
      • Spectral width 150ppm to -200ppm
      • 16 scans
      • Total time: 3 minutes
      • Recommended Concentration:  0.1mM
    • 1D Fluorine observe, 1H decouple 
      • Setup is exactly like direct observe 19F, only F2 is 1H and uses Waltz 16 decoupling.

About Us

The Research Instrumentation Facility (RIF) in the Department of Chemistry is equipped with a wide variety of instrumentation for chemical analysis including NMR, optical spectroscopy, thermal analysis and GC-MS. Our primary mission is to support the research within this department and the wider University system but we are additionally available to support the analytical chemistry needs of other academic institutions, research laboratories, businesses and individuals. We are available to run samples and compile data or reports as necessary.

RIF Picture

Facility Staff

Martha Morton
Martha Morton, Ph.D.
Director of Research Instrumentation
834 Hamilton Hall
(402) 472-6255
mmorton4@unl.edu
Thomas Smith
Thomas Smith
Assistant Director of Research Instrumentation
832B/414 Hamilton Hall
(402) 472-3797
tsmith@unl.edu
Jonathan Catazaro
Jonathan Catazaro
Graduate Student, Powers Group

Rates and Reservations

Make a reservation

Academic Rates: UNL Internal Users

Short Term
(0-4 hours)
Long Term
(4-24 hours)
Sampler Changer Rate
NMR 300 $9/hour $6/hour $8/hour
NMR 400/600 $9/hour $6/hour n/a
NMR 700-cryoprobe $20/hour $12/hour $12/hour
GCMS/UVvis/AA-Fluorimeter/IRmicroscope/HPLC-GC/CD $9/hour $9/hour $9/hour
Avatar_IR $20/hour $20/hour n/a
STA-Thermal Analysis $9/hour $9/hour n/a
ReactIR $20/day

Academic Rates: UNL External Users

Short Term
(0-4 hours)
Long Term
(4-24 hours)
Sampler Changer Rate
NMR 300 $18/hour $12/hour $16/hour
NMR 400/600 $18/hour $12/hour n/a
NMR 700-cryoprobe $40/hour $24/hour $24/hour
GCMS/UVvis/AA-Fluorimeter/IRmicroscope/HPLC-GC/CD $18/hour $18/hour $18/hour
Avatar_IR $40/hour $40/hour n/a
STA-Thermal Analysis $18/hour $18/hour n/a
ReactIR $40/day

Industrial Rates

Short Term
(0-4 hours)
Long Term
(4-24 hours)
Sampler Changer Rate
NMR 400/600 $110/hour $110/hour n/a
NMR 700-cryoprobe $150/hour $150/hour $150/hour
GCMS/UVvis/AA-Fluorimeter/IRmicroscope/HPLC-GC/CD $110/hour $110/hour $110/hour
Avatar_IR $110/hour $110/hour n/a
STA-Thermal Analysis $110/hour $110/hour n/a
ReactIR $200/day

Notes

  • Self operated rate is only available to academic customers after training is completed.
  • Training is only offered to academic customers and only when they are expected to have long-term consistent usage.
  • Discounts are available for industrial customers purchasing monthly blocks of time on a yearly basis.
  • NMR tubes, solvent and any other supplies consumed in acquiring data will be charged back to the customer for all samples.
  • For submitted samples any requested sample preparation, data work up and/or interpretation time will be charged at the above rate.
  • For submitted samples there is no minimum charge, only the actual time used will be charged in fractional hours.
  • State Sales tax will be added to all services and supplies for entities which are not tax exempt.
  • View official rates
  • Please direct any questions to Martha Morton