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NMR Laboratory

The DLSU NMR Laboratory is a full-service laboratory under the office of the DLSU Vice Chancellor for Research and Innovation. The facility operates a High Resolution JEOL 600 MHz NMR spectrometer located in Room GT101A Dr. George Ty Central Instrumentation Facility at DLSU Laguna Campus in Biñan, Laguna. The facility offers NMR Analytical Services and accepts samples not only from DLSU researchers but also from outside clients (academe, government, and industry) for a fee (please see schedule of fees). Interested users may also perform hands-on operation of the NMR after receiving proper training.

NMR Specifications

Jeol 600 MHz NMR: 14 Tesla Superconducting Magnet; 54 mm room temperature bore size; 10 to 600 MHz Frequency range; 2-Channel Amplifier System

Available Probes:

  1. Liquid Probe. Solution NMR holders: 3 mm and 5 mm NMR tubes
  2. Solid Probe (3.2mm HXMAS solid probe). Solid probe sample holder: 3.2mm Zirconia.

Auto shimming on deuterium, digital lock system, 24-slot auto sampler, and pneumatic sample lift and spinning

What can we offer?

The DLSU NMR Laboratory offers the following services:

  • Co-polymer analysis
  • Routine solution NMR analysis 1H, 13C, DEPT in full automation.
  • 2D NMR experiments: COSY, NOESY, ROESY, TOCSY, HMBC, HMQC, HSQC, etc.
  • Multi-nuclei NMR analysis within the frequency range of 19F, 31P, 29Si….. to 15N
  • More demanding multi pulse experiments such as nOe.
  • Dynamic, variable temperature experiments in the range -100 °C to +150 °C
  • Observation of traditional inorganic multinuclear analysis
  • Solid state NMR analysis of powder samples observing 1H, 31P, 7Li, 11B, 23Na, 27Al, 13C, 79Br, 207Pb, 29Si, 6Li, 15N nuclei.
  • Co-polymer analysis
How are samples prepared for Solution NMR analysis?

STEP 1. Ensure the sample is dry. Water and solvent peaks will appear in the NMR spectra.

STEP 2. Weigh the amount of the dry sample. To ensure quick analysis, the following are the recommended amounts:

2 – 10 mg for 1H NMR analysis

10 – 50 mg for 13C NMR analysis

10 – 20 mg for both 1H and 13C NMR analysis

Samples below these amounts will require longer scans.

STEP 3. Check the solubility of the sample. NMR analysis depends on the solubility of the sample in deuterated solvents. Choose the appropriate deuterated solvent for NMR analysis. The deuterated solvents listed in the schedule of fees may be available on stock. Please check with us on the availability of the deuterated solvent. Note that the use of solvents from our inventory will incur separate cost.

STEP 4. Check the relative purity of the sample. The quality of your analysis/interpretation will depend on the purity of the sample.  It is assumed that considerable effort has been done to purify the sample.

STEP 5. Pack the sample vials carefully for transport. We recommend to insert the samples in a DIY block styrofoam with holes enough to fit the vials.

STEP 6. Submit the sample to DLSU for analysis. Please click here on instructions how to submit the samples.

If you have an NMR tube and deuterated solvent, kindly prepare your sample following the protocol below. Otherwise, we will prepare the sample for you.

STEP 7. Add a small amount of deuterated solvent to the sample in the vial. The solvent volume should be enough to fill the required volume in the NMR tube. Mix the sample with the deuterated solvent properly.

  • Avoid contamination! Anything that comes in contact with the sample such as the Pasteur pipette, NMR tube, cap, solvent, etc. should be clean. Contaminant peaks will appear in the spectra.
  • The sample should be totally soluble in the deuterated solvent and should yield a clear solution. A turbid solution produces a poor spectrum.
  • The sample solution should be free of precipitate, dust, fibers, etc. Suspensions and opaque solutions will also yield a poor spectrum.
  • Samples that form two (2) phases with the solvent are not allowed.
  • Suspensions or precipitates in the sample should be filtered off.

STEP 8. Transfer the solution to the NMR tube using a disposable Pasteur pipette.

  • Do not dilute the sample in the tube with the solvent as it will result to a concentration gradient.
  • Avoid mixing the sample in the tube as it might be contaminated with the cap. Caps (even new ones) release materials when in contact with CDCl3 or DMSO-d6.
  • Insufficient volume of sample solution in the NMR tube will lead to a poor spectrum.
  • The volume of sample solution depends on the internal diameter of the NMR tube. A 5-cm sample depth in the NMR tube is required. A small amount of solvent yields a bad spectrum while large amounts dilute the sample (which leads to a poor spectrum) and wastes the solvent.

STEP 9. Label the NMR tube accordingly. Use a commercially-available sticker label and stick it to the top portion of the NMR tube concentrically. Secure the label with transparent tape.

STEP 10. Pack the NMR sample tube carefully for transport. We recommend to insert the samples in a DIY block styrofoam with holes enough to fit the tube.

STEP 11. Submit the sample to DLSU for analysis. Please click here on instructions how to submit the samples.

The following steps are to be done in the DLSU NMR lab by the NMR personnel or qualified student/researcher

STEP 12. Insert the NMR tube in the sample holder. Sample folders for 3 mm and 5 mm NMR tubes are available.

STEP 13. Check the required volume of the sample solution using the sample gauge.

STEP 14. Fill-up the logbook indicating the following: Account Name (name of faculty or principal investigator); student/researcher initials, sample code, slot number, solvent and experiment to be done. The slot number refers to the slot in the auto sample holder where you place the sample.

How do you submit samples for analysis?

STEP 1. Prepare the samples. Please see the sample preparation protocol. Options in submitting samples for analysis:

  1. If you don’t have NMR tubes and deuterated solvent: Send samples in a vial. Please follow sample requirements and sample preparation protocol. We will prepare the samples in NMR tube. Note that NMR tubes and deuterated solvents will incur separate costs.
  2. If you have NMR tubes and deuterated solvent: Prepare the samples in the NMR tube following the sample preparation protocol.

STEP 2. Fill up the NMR analysis form per sample. The form can be downloaded from the downloadable section.

STEP 3. Submit the analysis form together with the sample to the NMR personnel. To serve you better, we request a conference/discussion with you to help you determine the appropriate NMR experiments to achieve your objectives. Please e-mail us at [email protected] to confirm the conference/discussion schedule before going to DLSU.

Alternatively, electronic submission of forms and discussion can be accommodated through e-mail.

STEP 4. Submit the actual sample to the following venues:

  1. DLSU Taft Campus: DLSU Chemistry Department William Hall 501. Look for Dr. Drexel Camacho. Please call (02) 85244611 local 430.

Note that samples submitted at the DLSU Taft Campus have to travel to the DLSU Laguna Campus. The risk of breakage may occur during transit.

  1. DLSU Laguna Campus: Central Instrumentation Facility (Clean Building) at GT101A. Look for the NMR staff. Please coordinate with us through e-mail prior to your visit so we can have your gate pass processed.

STEP 5. Get the billing form. Billing forms can be requested ahead of time so that estimates can be made. Note however that requests for billing forms can only be accommodated if you know the number of scans you want for your analysis.

STEP 6. Proceed to the accounting office to pay for the analysis fees. Payments can be received at DLSU Laguna accounting offices. Cash and check payments are acceptable. Checks should be issued to: De La Salle University, Inc.

STEP 7. Please send a photocopy of the receipt to the NMR personnel for record keeping. Receipts are required before the results are released.

Frequently Asked Questions

Can I observe during the NMR analysis?
Yes. We can accommodate 1-2 observers. Please coordinate with us for the gate pass and schedule.
Is your NMR equipped with auto-sampler?
Yes. The NMR is equipped with an auto sampler and can hold up to 24 samples. It can be programmed for continuous analysis.
Do you offer rush analysis?
Yes. Rush analysis is available for twice the published rate. Please contact us for rush analysis at [email protected].
Do you process the spectra after the analysis?
Yes. We process the spectra and do integrations and expansions as we see fit. We send a pdf of the processed data through your e-mail. You can request for more detailed integrations and expansions.
Do you interpret the spectra after the analysis?
No. We don’t provide spectra interpretation.
Can you provide the ASCII data of the spectra after the analysis?
Yes. ASCII files, which can be inputted in Excel, can be requested and be sent to your e-mail for free.
Do you give the raw data after the analysis?
Yes. We can send the raw data (jdf file) through your e-mail. This requires a JEOL DeltaTM  software to be processed. A free trial version is available for download. Please visit the JEOL website for  details: https://www.jeol.co.jp/en/products/detail/Delta5.html
How long will you store the NMR results?
Results will only be retained for a period of 1 year after the date of analysis. All data will be deleted after the retention period.
Will you inform the clients before deleting their NMR data after the retention period?
No. It is the responsibility of the client to ask for additional copies of the data during the retention period.
Do you have lab space for lab works prior to NMR analysis?
Yes. For cases where laboratory space is required to do prior work (e.g. doing a reaction set-up for NMR monitoring of reaction), separate fees are required for the use of the lab and equipment. Please contact us for details at [email protected].
Do you offer block time usage?
Yes. We offer block time usage for NMR analysis at a discounted rate. Block time usage is offered to academic principal investigators/research groups by “blocking” the NMR time for their sample analysis after depositing a specific amount. Please contact us for details at [email protected].
Do you offer discounted rates for students?
Yes. Discounted rates are offered for accounts/research groups who signed a block-time usage with us. For more details, please contact us at [email protected].
Do you offer training for NMR usage?
Yes. Training for NMR usage is available. It is free for up to 5 persons for research groups with a block-time contract with us. Otherwise training is offered for a fee. Please contact us for details at [email protected].
Do you provide certification after NMR training?
Yes. Certificates can be requested after lecture type NMR training session. Certifications for the actual use of NMR require additional hands-on operation, monitored evaluation and examinations. As of the moment, these trainings are not yet qualified for CPD units.
Your contact information is not working, is there an alternative e-mail?
Contact us at these alternative e-mails: [email protected] , [email protected] , [email protected] or https://facebook.com/DLSUNMRLab/
Can we visit the NMR facility anytime?
As a university policy, all visitors should have a proper host inside the university while visiting. We require prior information before going to the DLSU Laguna Campus such as the full names of the visitors, date and time of the visit, car information such as the color, make and plate number.
Do you have parking space at DLSU Laguna?
Yes, parking spaces are available at DLSU Laguna. Please coordinate with us before coming for the gate pass. We need information such as the full names of the visitors, date and time of the visit, car information such as the color, make and plate number.
How can we go to DLSU Laguna?
For directions, you can use the Google Maps app or the Waze app and input “DLSU NMR Laboratory”.
From Manila by car, use the SLEX, exit at Sta. Rosa (or Eton), proceed to Paseo de Sta Rosa. At the intersection of Sta. Rosa-Tagaytay Road and Laguna Blvd, proceed to Laguna Blvd going to Laguna Technopark. Alternatively, you can exit at Mamplasan, and take the CALAX and exit at Laguna Technopark, then U-trun towards Laguna Technopark gate 2. After Laguna Technopark Gate 2, continue straight until you see a DLSU star signage (on the right). Turn left and pass under the CALAX road and continue straight until the rotunda. DLSU Laguna gate is at the second exit.
From Manila by public transportation. Take a bus going to Sta. Rosa. Get off after the Sta. Rosa exit toll gate. Take a tricyle going to Shopwise Paseo de Sta. Rosa. Hail a tricyle for a special trip to DLSU Laguna.
Do you have accommodation at DLSU Laguna for overnight stay?
There is a dormitory on campus that accepts transient stay. Please contact us for details at [email protected].

Downloadable Forms

NMR Analysis Form (doc)

NMR Analysis Form (pdf)