Statement of Requirement (Revised 3.28.22).pdf

STATEMENT OF REQUIREMENTS (Revised 3.28.22)

TITLE: Procurement of a 300 MHz solid-state NMR spectrometer

I. BACKGROUND INFORMATION

The Functional Polymers Group of the Materials Science and Engineering Division develops methods to spectroscopically characterize polymers that are used in technologically relevant devices such as fuel cells and water filtration membranes. Solid-state nuclear magnetic resonance

(NMR) spectrometers are used to determine structures at the atomic level. A new NMR spectrometer needs to be purchased that is capable of performing modern solid-state and diffusometry NMR experiments, which are critical for investigating the chemistry and physics of polymers important to the Functional Polymer Group’s mission. Although there are a variety of solid-state NMR consoles, not all of them can replace the current solid-state NMR spectrometer.

The current 300 MHz NMR spectrometer is a DMX300 spectrometer and includes an 89-mm bore UltraShield 7.05 T magnet and multiple 89-mm bore magic angle spinning (MAS) NMR probes for solid samples.

II. SPECIFICATIONS

The Contractor shall provide one (1) solid-state NMR spectrometer console and (1) pulsed field gradient probe that meets or exceeds the following minimum technical requirements. The

Contractor shall install the instrument and provide training as described below:

Base Line Items:

Hardware

1. The solid-state NMR spectrometer console shall be compatible with the current 7.05 T magnet (Bruker UltraShield 300 MHz/89 mm, p/n Z54957) and the following NMR probes:

• 1.3 mm solid-state NMR MAS probe

▪ Bruker p/n: PH MAS DVT 300 W1 BL1.3 N-P/H, s/n: H11313/0003

▪ ≤67 kHz magic angle spinning

▪ 30 °C to 70 °C

• 4 mm double resonance solid-state NMR MAS probe

▪ Bruker p/n: PH MAS 300 WB BL4 WVT, s/n: H7967/0023/00

▪ ≤15 kHz magic angle spinning

▪ -120 °C to 120 °C

• 4 mm triple resonance solid-state NMR MAS probe

▪ Bruker p/n: PH WB 73 MAS 4 BL CP Triple, s/n: H8845/0018/00

▪ ≤15 kHz magic angle spinning

▪ -120 °C to 120 °C

• 5 mm static wideline solid-state NMR probe

▪ Bruker, p/n PH WB 73A/BB SOL 5 BB HT

▪ No magic angle spinning

▪ -150 °C to 250 °C

• 5 mm single resonance solid-state NMR MAS CRAMPS probe

▪ Doty Scientific Inc., p/n DSI-774

▪ 0.05 kHz to 18 kHz magic angle spinning

▪ -150 °C to 250 °C

• 7 mm double resonance solid-state NMR MAS probe

▪ Bruker, p/n MAS 300 WB BL7 WVT, s/n: H8111/0019/00

▪ ≤7 kHz magic angle spinning

▪ -120 °C to 120 °C

• 5 mm solution NMR probe (Bruker, p/n BBI)

• 10 mm solution NMR probe (Bruker, p/n BBO)

2. The solid-state NMR spectrometer shall contain no fewer than four independent radiofrequency transmitters, 5 MHz (or lower) to 301 MHz (or higher) frequency ranges with fast phase switching (<15 ns); fast phase-continuous frequency switching (<25 ns) over an intermediate frequency (>20 MHz) range and capable of chirped pulses over a range of > 1 MHz; with phase stability and switching control to within 0.01º; timing stability and synchronization between all channels of no greater than 15 ns; no less than

64 million point waveform memory; and a minimum of 1 V output.

3. The solid-state NMR spectrometer shall include two or more independent digital receivers with >85 dB of gain capable of fast digital detection (<100 ns) and simultaneous detection of no fewer than two channels

4. The solid-state NMR spectrometer shall include two signal-averagers each with memory capable of acquiring multi-dimensional NMR spectra (≥1 GB of memory)

5. The solid-state NMR spectrometer shall include a deuterium lock channel, and a shim controller with at least 17 independent channels of ±1 amp, 5 amps maximum current for all channels with at least 18-bit computer control, and software matrixing. The shim controller shall be compatible with our current shims (Bruker DMX300) or the

Contractor will provide new shims for the shim controller.

6. The solid-state NMR spectrometer shall include one linear high power rf amplifier with maximum power of 1 kW or greater for 1H NMR for 300.13 MHz with ±1 MHz bandwidth (or greater) with 0.0003 ms (or less) to 100 ms (or greater) pulses and duty cycles ≥ 0.1 and with gain thermal stability to within ±0.01 dB/°C.

7. The solid-state NMR spectrometer shall include one linear high power rf amplifier with maximum power of 500 W or greater for 19F NMR for 282 MHz with ±1 MHz bandwidth

(or greater) with 0.0003 ms (or less) to 100 ms pulses (or greater) and duty cycles ≥ 0.1 and with gain thermal stability to within ±0.01 dB/°C.

8. The solid-state NMR spectrometer shall include two linear high power rf amplifiers with maximum power of 500 W or greater for frequencies 0.5 MHz (or less) to 150 MHz (or greater) with 0.0003 ms (or less) to 100 ms (or greater) pulses and duty cycles ≥ 0.1 and with gain thermal stability to within ±0.01 dB/°C.

9. The solid-state NMR spectrometer shall include a magic angle spinning (MAS) pneumatic system that can control MAS frequencies of 0.05 kHz to 67 kHz with no less than ±1.5 Hz accuracy and with MAS drift of no greater than ±1.5 Hz. Furthermore, the

MAS pneumatic system must:

• Allow for either manual or automated control of MAS rates

• Be capable of driving the sample eject/lift system in the sample exchangers compatible with our current probes (listed under Hardware #1) for safe, reliable, and stable changing of samples either manually or remotely.

• Include different settings for and be compatible with all five MAS NMR probes listed above (under Hardware #1), including providing the proper power supply to the optical tachometer, receiving the TTL pulses from the optical tachometer in any of the MAS probes above and, upon receiving the TTL signal, accurately controls the MAS probe input drive and bearing gas pressure to actively regulate the MAS rate given

• Accept 100 ± 1 p.s.i input gas

• Allow for user adjustable MAS acceleration and deceleration rates

10. The solid-state NMR spectrometer shall include a gradient amplifier for delivering gradient pulses with maximum amperage of 60 A or greater.

11. The solid-state NMR spectrometer shall include a single-axis pulsed field gradient probe capable of acquiring NMR data for 1H, 19F, 7Li, and 13C nuclei for 5 mm sample tubes over a wide range of temperatures (-70 °C to +110 °C). Furthermore, the pulsed field gradient probe shall:

• Include a electronically controlled recirculating water chiller for cooling the gradient coil

• Be capable of delivering either a continuous gradient (>180 G/cm) or pulsed gradients

(>1380 G/cm) with the 60 A amplifier for at least a 1.1% duty cycle

• Be capable of withstanding continuous current (≥ 7.5 A) or pulsed current (≥73 A) without breakdown

• Maintain gradient linearity to within less than 4% root mean squared deviation of the mean gradient over the sample tube diameter and less than 4% root mean squared deviation of the mean gradient over 12 mm of the sample tube length

• Be capable of slew rates between ≥2870 T/m/s

• Interface with the Bruker DMX300 sample exchange system for 5 mm tubes, or be provided with a sample exchange system equivalent to the Bruker DMX300 sample exchange system for 5 mm tubes, or be provided such that the Bruker 300DMX sample exchange system will be modified for proper interfacing.

12. The solid-state NMR spectrometer shall include a temperature controller that will control any temperature from -150 °C to 250 °C to within 0.2 °C (mean temperature) for experiments lasting up to four hours for any sample inside the (1) sample tube for any of the above non-MAS NMR probes, and (2) the rotor during magic angle spinning experiments for all of the above MAS NMR probes for experiments performed in the range 1 kHz to 18 kHz. Furthermore, the temperature controller shall:

• Allow for smooth transitions between temperature settings

• Include a heater shut-off safety mechanism for cases when air flow is interrupted to protect the probe from temperatures > 250°C

• Be able to control any temperature from -150 °C to 250 °C when using a liquid cryogen heat exchanging system and control any temperature from -20 °C to 250 °C when using a non-cryogen-based chiller system that does not require manual filling of cryogens. Furthermore, the chiller must:

o operate with dry air input gas with a dew point of -73 °C up to pressures of

100 p.s.i. for over 7 days at a time without interruption o provide at least 2 cubic feet of chilled gas per minute for temperatures -20 °C or lower for over 7 days at a time without interruption.

o be controllable via the computer software.

o cool MAS samples in our 4 mm triple resonance MAS probe (Bruker, PH WB

73 MAS 4 BL CP Triple) for any MAS rate between 1 and 18 kHz and maintain

MAS stability to within ±1.5 Hz.

o cool MAS samples in our 5 mm single resonance CRAMPS probe (Doty

Scientific Inc., p/n DSI-774) for any MAS rate between 1 and 7 kHz and maintain MAS stability to within ±1.5 Hz.

o cool MAS samples in our 7 mm double resonance MAS probe (Bruker, p/n

MAS 300 WB BL7 WVT) for any MAS rate between 1 and 7 kHz and maintain

MAS stability to within ±1.5 Hz.

o allow for transitions between temperature settings without disrupting magic angle spinning.

13. Software and hardware that can read the helium level in our magnet using our current helium sensor. The current Bruker magnet system is # 300/89LL US D205, part #

Z54957/0008, coil # BZH 08 30 107B, dewar # D 205/89-3050. The helium sensor type is 1300/700.

Computer/Software

14. The solid-state NMR spectrometer shall include a computer with software that controls all aspects of the spectrometer, including the timing and amplitude of all rf pulses and gradient pulses, triggers, receiver acquisition, sample temperature, magic angle spinning rate, and reading/displaying the magnet’s helium level using the current helium sensor.

15. The computer shall have at least 1 TB (or greater) of disk space and 16 GB (or greater) of memory, will be fast enough (>2 GHz processor) to be capable of processing NMR data for analysis in up to 4D, will be compatible with automated looped and/or block acquisition of multiple experiments, and allow for remote operation of the spectrometer.

The spectrometer computer shall include software for acquiring PFG data, possess memory sufficient for processing the PFG data via inverse Laplace transform (processing within the software is optional), and represent spectral data in multiple dimensions (when needed) for interpretation.

16. The spectrometer shall have safety monitoring systems that are capable of monitoring, shutting down, and warning the user if errors occur in the operations of the spectrometer during an experiment, including rf or gradient pulsing errors, receiver errors, overheating, or MAS errors, thereby protecting the integrity of the data and the spectrometer hardware.

17. The computer shall have built-in macros that can acquire NMR spectra

• from multiple experiments in a set determined by the user, and loop to the first experiment for additional signal averaging and continue with the rest of the experiments in the set, for any number of loops from 1 to 100,000, or any number of scans from 1 to 100,000,000;

• that can be added to or written over previously acquired spectra upon initialization of the experiment;

• upon manual initialization or initialization by an external TTL pulse;

• that can be automatically saved after the end of an experiment.

In addition, the spectrometer shall be compatible with the following items of existing equipment or provide the new equipment to fulfill the requirement

Requirement Existing equipment

(1) Pneumatically driven sample exchange tubes for 4 mm MAS, 7 mm MAS, 5 mm BBI, and 10 mm BBO probes

Sample exchange tubes in Bruker DMX300 including:

4 mm MAS (p/n: AS Trans WBHT BL4 100-400)

7 mm MAS (p/n: AS Trans WBHT BL7 100-400)

5 mm solution probe (p/n: BBI)

10 mm solution probe (p/n: BBO)

(2) 17 channel room temperature shims

Shims with Bruker DMX300 (s/n: 37825)

(3) Liquid nitrogen heat exchanger Liquid nitrogen heat exchanger with Bruker DMX300

(4) Uninterruptable power supply to protect the console and allow the spectrometer to run continuously during power spikes and outages for > 1 minute

10 kVA Liebert NX, three phase

Optional Line Items:

• Micro-MRI equipment

Two additional high amperage ≥50 A gradient amplifiers (≥55 A peak current) and a triple-axis microimaging probe capable of acquiring NMR data for 1H, 7Li, 13C, 23Na, 31P and 35Cl (19F optional) nuclei over a wide range of temperatures (-40 °C to +80 °C) for 10 mm sample tube diameters, which shall:

• be capable of delivering either a continuous gradient (≥24 G/cm) or pulsed gradients (≥240

G/cm) with the ≥50 A amplifier for at least a 1.1% duty cycle

• be capable of withstanding continuous current (≥5 A) or pulsed current (≥73 A) without breakdown

• maintain gradient linearity to within less than 4% root mean squared deviation of the mean gradient over the sample tube diameter and less than 4% root mean squared deviation of the mean gradient over 16 mm (or greater) of the sample tube length

• be capable of slew rates of 1150 T/m/s or greater

Installation:

The Contractor shall install the instrument in Building 224, Room B125 or B325, at NIST

Gaithersburg, MD. Installation shall include, at a minimum, uncrating/unpacking of all equipment, set-up and hook-up of all equipment, start-up, demonstration of specifications, and removal of all trash. Instrument will operate to manufacturer’s specifications upon installation.

Installation will take place during normal business hours, between 8:30 am and 5:00 pm Eastern

Time, Monday through Friday except Federal Holidays, and will be coordinated with the NIST

Technical Point of Contact (TPOC). Installation shall occur within 14 calendar days after receipt of instrument.

Warranty:

The Contractor shall provide, at a minimum, a one-year warranty for the equipment. The warranty shall cover all parts, labor and travel. The warranty shall commence upon successful completion of delivery, installation, training and demonstration of all required specifications.

Training:

Include training at NIST for up to 2 NIST personnel covering normal operation, troubleshooting, and routine maintenance. Training will be provided during normal business hours, between

8:30am and 5:00pm Eastern Time, Monday through Friday, except Federal Holidays, and will be coordinated with the NIST Technical Point of Contact (TPOC) to ensure maximum availability of NIST personnel. Training is to occur within 10 calendar days of installation. The training shall be completed on-site at NIST immediately after installation and demonstration of specifications.

III. DELIVERY

The contractor shall deliver the equipment, FOB Destination shipping terms to the following addresses:

Ryan Nieuwendaal

National Institute of Standards and Technology

100 Bureau Dr.

Building 224

Gaithersburg, Maryland 20899-8371

IV. DELIVERABLES

Description Quantity Due Date

BASE LINE ITEMS:

300 MHz solid-state NMR spectrometer console

One (1) 120 calendar days after award

Installation of the 300 MHz solid-state

NMR spectrometer console

Once* 14 calendar days after receipt of instrument

Operations and maintenance manual for the

300 MHz solid-state NMR spectrometer console

One (1) 120 calendar days after award

Training of NIST personnel at NIST, Gaithersburg, MD

Once* 10 calendar days after installation.

OPTIONAL LINE ITEMS:

Micro-MRI equipment One (1) 120 calendar days after award

* Multiple installation/training periods of components of the spectrometer (console, pulsed field gradient probe, triple-axis pulsed field gradient probe) will be acceptable if they speed up delivery and are all completed within 120 days of receipt of award.

V. ACCEPTANCE CRITERIA

After installation, the TPOC shall coordinate with the Contractor to test and demonstrate that all minimum required specifications have been met. The demonstration of specifications may occur during training. Final acceptance by the Government will be given after successful delivery, installation, training, and demonstration of instrumentation specifications, including the following acceptance tests:

1. On a 20 mg standard sample of adamantane a 13C NMR spectrum can be collected with a signal-to-noise ratio of 120:1 (39 ppm resonance) with 16 Hz baseline resolution when using the 1H-13C cross polarization sequence ( CB1 = 60 kHz, HB1

= 48 kHz, 6% 1H ramp) and 1H

TPPM decoupling ( HB1 = 79 kHz) while magic angle spinning (12000 ± 1 Hz) with a 3 sec.

repetition time when using our triple resonance MAS probe (Bruker, PH WB 73 MAS 4 BL

CP Triple). Other relevant parameters are: 8 scans, 8 ms contact time, 2.95 s 1H /2 pulse at attenuation factor of 8.0, 20 ms dwell time, 4096 data points, 32 receiver gain.

2. On a 20 mg sample of adipic acid a 1H NMR spectrum can be collected with a signal-to-noise ratio of 250:1 (2 ppm resonance) with 2 ppm baseline resolution when using the

MREV-8 pulse sequence ( HB1 = 167 kHz) while magic angle spinning (2.5 kHz) with a 7 sec.

repetition time when using our 5 mm single resonance CRAMPS probe (Doty Scientific Inc., p/n: DSI-774) or similar CRAMPS probe provided by the vendor (for testing purposes only).

Other relevant parameters are: 19.6 s cycle time, 0.49 scaling factor, 8 scans, 8 second repetition time.

3. On a sample of poly(dimethyl siloxane) the transmitter gain values for /2 and pulses used in the multiple pulse tune-up sequence (D. P. Burum, et al. J. Magn. Reson., 1981, 43, p. 468, https://doi.org/10.1016/0022-2364(81)90058-5) do not change by more than 0.01 dB for every 1 °C change in temperature of input gas blown into the amplifier when using our 5 mm

CRAMPS probe (Doty Scientific Inc., p/n: DSI-774) or similar CRAMPS probe provided by the vendor (for testing purposes only).

4. A 1H NMR spectrum of 180 L of chloroform can be acquired with a full-width-at-half-maximum linewidth of 2 Hz using the NIST 5 mm BBI probe.

5. A 1H NMR spectrum of 180 L of 0.1% ethyl benzene (in chloroform) can be acquired with a signal-to-noise ratio of 70:1 (or greater) and a full-width-at-half-maximum linewidth of 2

Hz or less with a /2 pulse of 8 s or less for 20 W of input power or less after 1 scan when using the pulsed field gradient probe.

6. On a sample of lead nitrate using a full 4 mm rotor under magic angle spinning, the 207Pb chemical shift corresponds to the appropriate temperature as shown via A. Bielecki, et al. J.

Magn. Reason. A, 1995, 116(2), 215-220, https://doi.org/10.1006/jmra.1995.0010, for any temperature selected in the range of -120 to 120 °C with ±0.2°C accuracy when using a liquid nitrogen heat exchanger or any temperature selected in the range of -20 to 120 °C with

±0.2°C accuracy when using a non-cryogen-based chiller for a time period of one hour with less than 1°C of drift when using our triple resonance MAS probe (Bruker, PH WB 73 MAS

4 BL CP Triple).

7. NMR PFG diffusion curves acquired using the Stejskal-Tanner pulse sequence in the PFG probe measure the diffusion coefficients on the appropriate samples listed in Table 1 for the temperatures listed.

8. Optional: NMR PFG curves acquired using the Stejskal-Tanner pulse sequence in the https://doi.org/10.1016/0022-2364(81)90058-5 https://doi.org/10.1006/jmra.1995.0010 microimaging-MRI probe measure the diffusion coefficients on the appropriate samples listed in Table 1 for the temperatures listed for all three gradient axes.

The acceptance tests # 1, 2, 3, and 5 can be performed using either the NIST probes (Section II, line 1) or on probe(s) provided by the vendor to demonstrate the spectrometer specifications. If the vendor and TPOC determine that the NIST probes (listed in Section II.1) are not within their specifications (listed in their respective manuals) during the acceptance testing, alternative tests that are acceptable to the TPOC and vendor can be performed as a suitable replacement.

Table 1: Testing samples for PFG diffusion curves

Sample Probes Nucleus Temperature

(K)

Diffusion

Coefficient

(m2/s)

Single axis

PFG

(Sec. II, line

11)

Triple axis

PFG

(optional line item)

Water x x 1H 278 1.3 x 10-9

Water x x 1H 298 2.2 x 10-9

Water x x 1H 323 4.0 x 10-9

Poly(ethylene oxide) (Mw = 9 x

105 g/mol) in water

(0.05 wt% in D2O) x 1H 298 6 x 10-12

LiCl (0.25 M in

H2O) x x 7Li 298 9.6 x 10-10

Cyclohexane x x 13C 298 1.4 x 10-9

NaCl (2 M in H2O) x x 23Na 298 1.1 x 10-9

VI. GENERAL INFORMATION

Safety: The Contractor employee shall be responsible for knowing and complying with commercial installation safety prevention regulations. Such regulations include, but are not limited to, general safety, fire prevention, and waste disposal.

Security: NIST is a restricted campus. An identification badge is required for access for entry into buildings and also is shown to the armed Security Police when entering the campus.

Identification Badges: Contractor employees shall comply with NIST identification and access requirements. The Contractor shall provide the name and citizenship information of employees for on-site visits to the NIST Contracting Officer Representative (COR) prior to arrival. The

COR will submit the name(s) and citizenship information to the NIST Office of Security in order for a given Contractor employee to enter the NIST campus. The Contractor employee is responsible for absences due to missing or expired identification and access documents. Each

Contractor employee shall wear a visible identification badge provided by the NIST Security

Office.

Vehicle Registration: All Contractor employees must register their vehicles with the NIST

Security Office to gain access to the campus. A valid driver’s license, Government-furnished civilian ID (which in most cases can be a valid driver's license), proof of insurance and current registration must be presented to the NIST Security Office.