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Category
- Spectroscopy and Spectrometry » NMR Spectroscopy
Booking Details
Facility Management Team and Location
Facility Features, Working Principle and Specifications
Facility Description
The Bruker AVANCE NEO 400 MHz OneBay FT-NMR Spectrometer is a high-performance system designed for advanced research in organic, inorganic, bio molecular, and solid-state NMR. Featuring a 9.4 T superconducting magnet, AVANCE NEO console, and automatic tuning and matching (ATM), it delivers high-resolution spectroscopy with optimized cryogen efficiency.
Features:
High-Resolution Spectroscopy: Detailed atomic-level analysis of solid materials.
MAS (Magic Angle Spinning): Rotates samples to average anisotropic interactions, improving resolution.
CP-MAS (Cross-Polarization): Enhances sensitivity, especially for low-gamma nuclei like ¹³C.
Variable Temperature (VT): Enables temperature-dependent experiments.
Superconducting Magnet (9.4 T): Provides a stable magnetic field for precise measurements.
Efficient Cryogen Management: Low helium and nitrogen consumption.
Working Principle:
NMR measures how magnetic nuclei in a sample resonate with an external magnetic field, revealing structural and electronic properties.
MAS averages interactions to improve resolution.
CP transfers polarization from abundant nuclei (¹H) to less sensitive ones (¹³C, ²⁹Si).
Provides high-resolution spectra of solid materials, with temperature-dependent capabilities for studying molecular dynamics and reactions.
- Operating Frequency: 400 MHz for 1H (other nuclei operate at corresponding frequencies).
Probes:
- Liquid-state: i probe.
- Solid-state: MAS probe with a maximum spinning speed of 14 KHz.
Instructions for Registration, Sample Preparation, User Instructions and Precautionary Measures
1: Submit an Official Request Letter
- The letter must be on your institution's official letterhead.
- It should be signed by the Head of Department (HoD) or Research Guide.
- The letter must confirm that the analysis is for research purposes (to qualify for academic concessions).
2: Address the Letter To
The Head, Department of Chemistry, IIT Bombay.
3: Include the Following Details in the Letter
For Solid-State NMR Analysis:
- Type of Solid-State NMR Analysis Required
- Specify the nucleus of interest (e.g., ¹³C, ²⁹Si, ³¹P, etc.).
- Expected Spectral Range
- Mention the required frequency or chemical shift range.
- Any Special Requirements
- Mention if you need:
- Variable Temperature (VT) Experiments
- Cross Polarization Magic Angle Spinning (CP-MAS)
- Any other advanced techniques.
- Mention if you need:
For Solution-State NMR Analysis:
- Type of Solution NMR Analysis Required
- Mention the nuclei for analysis (e.g., ¹H, ¹³C, ³¹P, ¹⁹F, etc.).
- Type of Experiment Required
- Specify the required experiment (e.g., 1D NMR: ¹H, ¹³C, DEPT, APT, or 2D NMR: COSY, NOESY, HSQC, HMBC, DOSY, etc.).
- Sample Details
- Provide details such as:
- Solvent Used (e.g., CDCl₃, D₂O, DMSO-d₆, etc.)
- Sample Concentration
- Any Special Handling Requirements
- Provide details such as:
For Solid Samples:
- Ensure the sample is completely dry and finely powdered for optimal results.
Required Sample Amounts:
4 mm MAS rotor → 150–200 mg of sample.
- The sample must be non-magnetic and non-conductive (unless explicitly approved).
Special Instructions for Sample Handling:
Avoid hygroscopic samples unless pre-dried and handled under inert conditions.
Ensure there are no volatile solvents or moisture present in the sample.
If submitting air-sensitive samples, discuss the procedure with facility staff beforehand.
Liquid Samples:
- Ensure complete solubility in 0.6 mL of the selected solvent.
- Required amounts:
- 1H NMR: 10-20 mg (depending on molecular weight).
- 13C NMR: 20-30 mg for adequate signal-to-noise ratio.
For Solid-State NMR Analysis
Before Using the Facility:
- Familiarize yourself with the instrument manual and Standard Operating Procedures (SOPs).
- Check the compatibility of the sample with the MAS rotor and confirm its stability under spinning conditions.
During Experiments:
- Use the appropriate rotor and ensure the sample is packed properly.
- Handle the rotors carefully to prevent cracking or damage.
- Do not exceed the recommended spinning speed for the rotor type.
After Using the Facility:
- Ensure rotors and caps are returned in good condition.
- Report any issues to the lab personnel immediately.
- Collect spectra and retrieve any unused sample material, if needed.
For Solution-State NMR Analysis
Before Using the Facility:
- Read and understand the instrument manual and SOPs.
- Prepare the sample in a deuterated solvent (e.g., CDCl₃, D₂O, DMSO-d₆) to ensure proper locking and shimming.
- Filter the sample, if necessary, to remove insoluble particles that could interfere with the experiment.
- Use a clean and undamaged NMR tube with the correct length and thickness.
During Experiments:
- Handle NMR tubes carefully to prevent breakage.
- Insert the NMR tube gently into the spinner to avoid misalignment.
- Do not exceed the recommended sample volume (typically 0.6 mL for standard 5 mm tubes).
- Ensure proper shimming and tuning before starting data acquisition.
After Using the Facility:
- Remove the sample from the spectrometer and clean any spills.
- Collect your NMR spectra and save the data for future reference.
- Retrieve your unused sample material and dispose of waste properly.
Report any instrument issues or irregularities to the lab personnel.
Important Note for External Users:
- External users are NOT allowed to operate the instrument.
- Only authorized facility personnel will handle the sample preparation, experiment setup, and data acquisition for external users.
- External users must submit their samples along with a properly filled analysis request form and the required payment (if applicable).
- Users will receive the processed data once the analysis is complete.
Charges for Analytical Services in Different Categories
Expt. type | Internal | University (X) | National Labs (3X) | Industries (5X) | |
| Chemistry Dept. | Other IITB Departments (X) |
|
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|
1H | 50 | 100 | 100 | 300 | 500 |
X-nuclei | 50 | 200 | 200 | 600 | 1000 |
Subsequent hour | 50 | 150 | 150 | 450 | 750 |
2D NMR | 50 | 300 | 300 | 900 | 1500 |
Solid State | 50 | 1000 | 1000 | 3000 | 5000 |
Subsequent hour | 50 | 625 | 625 | 1875 | 3125 |
Additional Charges for Variable temp. (Solution/Solid) | 50 | 250 | 250 | 750 | 1250 |
Applications
Major application of NMR spectroscopy lies in the area of synthetic organic chemistry, inorganic chemistry, bio-organic chemistry, bio-inorganic chemistry, polymer chemistry and organometallic chemistry. One of the main advantages of FT-NMR spectroscopy is that a number of FIDs can be accumulated and Fourier transformed, enhancing S/N ratio of the spectrum. This in turn facilitates the analysis of samples with low abundant nuclei and smaller gyro-magnetic ratios, e.g.,13C, 29Si, 15N etc.
NMR studies find applications in some of following areas:
Molecular conformation in solution
Quantitative analysis of mixtures containing known compounds
Determining the content and purity of a sample
Through space connectivity (Overhauser effect)
Sample Details
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