Multi frequency electron paramagnetic resonance spectroscopy
Multi frequency electron paramagnetic resonance spectroscopy
Make
Bruker
Model
EMXplus
Facility Status
Working
Facility Management Division
Institute Central Research Facilities (ICRF)

Category

  • Spectroscopy and Spectrometry ยป ESR Spectroscopy

Booking Details

Booking available for
Internal and External Both
Available Mode for Use
X-band measurement at R.T. and 100K
Q-band measurement at R.T. and 100K

Facility Management Team and Location

Faculty In Charge
Prof. Gopalan Rajaraman
Facility Operator
Mr. Nitin Kadam <br>Mr. Narendra Gaikwad
Co-convenors
Prof. Gopalan Rajaraman
Prof. Maheswaran S.
Prof. R Murugavel
Department
Chemistry
LAB Email ID
mfepr.chem@iitb.ac.in
Facility Location
Building adjacent to Chemistry Department, Behind Security Kiosk (Ground floor)
Lab Phone No
02225764132

Facility Features, Working Principle and Specifications

Features Working Principle

Features

  • Variable temperature EPR (X and Q-band) measurement(5K-300K)
  • Single crystal measurement
  • Finger dewarn A
  • Working Principles
  • An EPR experiment the field of the spectrometer magnet is swept linearly to excite some of the electrons in the lower energy level to the upper energy level while the sample is exposed to fixed microwave irradiation. The free or the upaired electrons have a small magnetic field and orient themselves parallel to the larger field produced by the spectrometer's magnet. At a particular magnetic field strength the microwave irradiation will cause some of the free electrons to "flip" and orient against the spectrometer's magnetic field. This separation between the lower and the higher energy level is exactly matched by our microwave frequency. The condition where the magnetic field and the microwave frequency are "just right" to produce an EPR resonance (or absorption) is known as the resonance condition is detected by the spectrometer.
  • Digital Ultra High Resolution Hall Field Controller
    Microwave Bridge: Type EMX-m40X(X-band)
    Source: solid state microwave source;
    Frequency range: 9,3 to 9,9 GHz
    low noise: -130dBc/ 100 kHz from carrier
    maximum source output : 200mW
    phase sensitive detection
    integrated frequency counter with 1 kHz resolution

    Frequency Tuning:
    tune bandwidth: 8 MHz,
    suitable for standard resonator types
    Automatic Frequency Control(AFC):
    AFC lock range: 4 MHz
    digital adjustment for modulation amplitude and gain
    AFC stability: 10-8

    Microwave Power Setting:
    Attenuation : 60dB max
    automatic phase correction over attenuation range,

    Microwave Reference Arm:
    Reference Arm with microwave attenuation and phase shifter,

    Signal Amplifier: low noise preamplifier,
    20 Hz to 600 kHz,
    two 50 Ohm signal outputs

    Resonator Tuning and Matching:
    the system features "auto tuning" and "auto matching"
    for most probeheads via iris

    Q-factor Display:
    the system evaluates the probehead (resonator) and
    displays the loaded Q-Factor.
    All parameters of the bridge are software controlled

    High Sensitivity Probe (Type 2)
    with optical window for CW-EPR in X-Band:
  • 10 mm sample access
  • 20 G maximum modulation amplitude
  • automatic cavity matching
  • forlossy and non-lossy samples
  • compatible with ER 4131VT and ER 4112HV
  • unloaded Q > 15.000
  • Sensitivity: Weak Pitch 1200 : 1 Absolute 2.5 x 109 spins / G

  • Q-Band Microwave Bridge with frequency counter
    microwave source: Gunn
    Operating frequency: 34 GHz
    max. Power: 100 mW
    operating range: 100 MHz
    attenautaion precision: +/- 0.2dB
    attenuation resolution: 1 dB
    attenuation max.: 60 dB
    Signal bandwidth: 30 Hz to 400 kHz
    Integrated frequency counter with 1 kHz resolution

    ER 5106QT
    Cavity for room-, nitrogen, helium temperatures (X-band)

    Helium Cryostat, 3.8 K to 300 K (Q-band)
    with 5 mm optical window,compatible with ER 4112HV-1020 control system(including cryostat holder), used for Flexline,K- and Q-Band resonators.

    ER 5106QT
    Electrolytic cell assembly (X-band)
    Single crystal EPR measurement One axis Goniometer

Instructions for Registration, Sample Preparation, User Instructions, Precautionary Measures and Charges

Instructions for Registration
  • Internal users can register online.
  • External users need to down load registration form and submit it to lab along with the requisite demand draft. The samples should be submitted personally on the day of allotted time slot. Analysis will be performed on the next day and results will be sent through email.
  • Getting back the samples: Users desiring to get back the samples need to mark on the form. Collect them from the lab between 9:30 AM to 11:00 AM after two-three days of completion of the work (intimated through mail) and uncollected samples will be disposed off after ten days of intimation of the completion of the work and no reminders will be sent.
Instruction for Sample Preparation
  • For X-band:
    • Minimum 40-50 mg sample is needed for solid state measurement
    • For solution state measurement 1 x 10-2 M (provide the preferable solvent to dissolve your sample (avoid using highly polar solvent for measurement))
  • For Q-band:
    • Minimum 5-20 mg sample is needed for solid state measurement
    • For solution state measurement 1 x 10-3 M (provide the preferable solvent to dissolve your sample (avoid using highly polar solvent for measurement))
User Instructions and Precautionary Measures
  • Registered user will be allotted time as per queue.
  • User should submit the samples to the EPR lab between 9:30 AM and 11:00 AM on the scheduled day.
  • Samples will be loaded in to the system on the submitted day and analysis will be carried out after 4 to 6 hours or on the next day. Data will be sent through email.

Applications

  • Interaction between the unpaired electron in the system (Organic or Inorganic complexes)
  • To find out the geometry around metal ions (particularly useful in biology Example: active site of enzymes and metalloproteinase)
  • EPR imaging
  • Radicals trapping
  • Probing the radical mechanism of chemical and biological catalysis reaction
  • To probe mechanism of Radical polymerization
  • Spin labelling experiments
  • Quantitative absolute concentration measurements

Sample Details

SOP, Lab Policies and Other Details

Publications

Publications
NA