400-1

Fully automated with a 60-sample autosampler, 400-1 provides the most convenient way to obtain routine NMR spectra in Searle. Equipped with a Bruker “Smart” BBFO probe with automated tuning, this instrument acquires high-quality spectra with a wide variety of experiments, including 2D (COSY, HSQC, HMBC), and heteronuclear 1D (¹³C, ³¹P, ¹⁹F, ¹¹B, and more) – each sample requiring only a minute or two to set up. Researchers with special privileges are allowed to run “intermittent” kinetics experiments, in which short spectra of a sample containing an ongoing reaction are acquired on a near-regular schedule for several hours or days.

Researchers use 400-1 in three popular ways:
• Running several samples (~2-6) at once, supporting research in synthetic methodology
• Conveniently acquiring multiple characterization spectra at night, e.g. ¹H, COSY, HSQC, HMBC, long ¹³C
• Providing focus on data analysis, not mechanics of acquisition – perfect for infrequent users

Console

• Bruker Avance III HD 400 MHz Nanobay
• 2-channel, Z-gradient
• Manufactured 2016, installed 2017

Default Probe

• Bruker BBFO “Smart” probe
• Inner coil (more sensitive) = ¹⁰⁹Ag – ¹⁹F
• Outer coil = ¹H
• Z-gradient
• ATM automated tuning module
• Manufactured 2016; installed 2017

Magnet

• Bruker Ascend 9.4 T / 400 MHz
• 5-gauss line within the magnet legs
• Liquid helium hold time 300 days
• Manufactured 2016; installed 2017

Auto-
sampler

• Bruker SampleCase Plus
• 60 samples
• Manufactured and installed 2020
• Handles all NMR tubes less than 222 mm (8.75″) long (including valved tubes, e.g. WILMAD 528-LPV-200M and NEW ERA NE-CAV5-135).

500-2

This is the instrument preferred for intensive experiments such as variable temperature (VT), titrations, reaction monitoring, customized 2D, etc. Reservations are required for overnight blocks or sessions up to 5 hours. When not in use or reserved, it is available for unreserved walkup use (< 20 min).

500-2 is the only spectrometer in Searle available for VT experiments, which require a short training session to perform. Researchers must schedule VT training with the facility manager before reserving time for VT experiments.

Console

• Bruker Avance III HD 500 MHz
• 3-channel, XYZ-gradients
• Installed in Searle 2014

Default Probe

• Bruker BBFO “Smart” probe
• Inner coil (more sensitive) = ¹⁰⁹Ag – ¹⁹F
• Outer coil = ¹H
• ATM automated tuning module, Z-gradient
• Temperature range: -150 °C to +150 °C

Magnet

• Bruker Ultrashield Plus 11.7 T / 500 MHz
• Liquid helium hold time 150 days (extra-long)
• Manufactured 2006
• Installed in Searle 2009

Low-temp accessory

With this liquid nitrogen-based system, samples can be cooled to as low as -150 °C for low-temperature NMR analysis. Training in its use is required. Researchers needing low-temperature operation on 500-2 must contact the facility manager to arrange for a 15-minute training session.

500-1

This is the preferred instrument for synthetic chemists in Searle who need rapid access to a manually-operated spectrometer so they can quickly assess reaction outcomes and make immediate decisions about their project’s next steps. Each session is limited to 20 minutes, and reservation are not required. Default parameter sets for essential 1D and 2D experiments are provided with that time limit in mind, ensuring maximum productivity.

Console

• Bruker Avance III 500 MHz
• 4-channel (including ²H)
• XYZ-gradients
• Installed in Searle 2012

Default Probe

• Bruker BBO probe
• Inner coil (more sensitive) = broadband (¹⁰⁹Ag – ³¹P) – no ¹⁹F
• Outer coil = ¹H (no ¹⁹F)
• Z-gradient
• ATM automated tuning module

Magnet

• Bruker Ultrashield Plus 11.7 T / 500 MHz
• Liquid helium hold time 150 days (extra-long)
• Manufactured 2006; installed in Searle 2009

Support Lab

The Searle NMR facility includes a small support lab equipped with a fume hood, bench, sink, flammables cabinet, and solvents cabinet. It’s perfect for conducting titrations or starting reactions to be monitored by NMR. Mixing chemicals and preparing samples is not allowed on the magnet floor, so having this resource here means researchers do not need to exit the facility and return to their own labs every time a sample needs a chemical adjustment.

Policy

The support lab operates on a “pack-it-in-pack-it-out” policy. The facility supplies no consumables and handles no waste. Researchers must bring their own materials (pipettes, gloves, safety glasses, small waste containers, etc.), usually in a plastic tray, and must leave the room as they found it, taking their hazardous waste with them.