National Institutes of Health, National Heart, Lung, and Blood Institute, Contracts Operations Branch, Procurement Section, 6701 Rockledge Drive, Room 6143, Bethesda, Maryland 20892-7902

66 -- CONSOLE UPGRADES TO NUCLEAR MAGNETIC RESONANCE SPECTROMETERS SOL NHLBI-HL-P-97-111 DUE 081197 POC Kathleen J. Van Steelant, Contracting Officer, (301) 435-0364 It is the intent of the National Heart, Lung, and Blood Institute e (NHLBI), Division of Intramural Research, Laboratory of Biophysical Chemistry, to acquire console upgrades to Nuclear Magnetic Resonance Spectrometers. The upgrades must meet the following minimum specifications: 600 MHZ: 1) The upgraded console shall be capable of operating at or above 600 MHZ 1H (proton) frequency and in the range of at least 30 -- 243 MHZ (with 15 -- 320 MHZ being preferable) for X nuclei up to and including 31P. Thi s upgraded console shall be interfaced with the existing Oxford magnet, upper and lower shim stacks, and existing probes and related hardware or the necessary modifications, replacements or substitutions made (at the discretion and approval of the project officer) to this existing equipment in use such that the working spectrometer (console, probes, interfaces, magnet, computers and related hardware devices) is identical in all respects (except for age of hardware not actually replaced) to spectrometers cur rently being marketed by the manufacturer. The Contractor shall take full responsibility for the entire system, including probe heads, shim system and superconducting magnet; 2) The upgraded console shall be equipped with and use a minimum of 28 room temperature shim gradients optimally designed for the highest magnetic field strength homogeneity commensurate with minimal heating. The upgraded console shall have the capability to perform computer controlled automated shimming of the magnetic field. Adjus tment of the superconducting magnetic field strength or shims required to obtain optimal room temperature specifications and shim performance shall be the responsibility of the Contractor and shall be carried out after consultation and in accord with the project officer; 3) The upgraded console shall have the capability to perform inverse detection NMR experiments for X frequencies in the range specified in 1 above; 4) The upgrade shall include a power supply capable of generating simultaneously and indepen dently power to drive three orthogonal gradients in three axis gradient probes. The shape, amplitude, duration and polarity of these gradients shall be under pulse program control and the use of various waveforms including sine shall be possible. Gradient amplifiers shall employ eddy current compensation and be linear, low noise, and preferably constant current. This system shall be capable of generating a field gradient along the z axis (axis of the magnetic field) with a strength of at least 25 G/cm on the 5-mm probe head(see next item). Gradients in the x and y dimensions of the three-axis probe shall be at least 25 G/cm. The vendor shall describe in detail in their proposal their strategy and procedure, including automation when applicable, for performing gradient shimming (magnetic field mapping). The vendor shall optimize the homogeneity of the region sampled by the 1H coil in e (below) including mapping of the field using gradient techniques on the existing 600 MHZ Oxford magnet in the buyer's la boratory; 5) The system shall include a triple resonance 5-mm three-axis pulsed field gradient probe for observation of 1H while decoupling 13C and 15N, include 2H lock, and the 90o pulse widths must be < 10 5s for 1H for an aqueous non ionic sample, < 15 5s ( 12 5s is preferred) for 13C for an aqueous non ionic sample, and < 44 5s ( 35 5s is preferred) for 15N for an aqueous non ionic sample. The probe head shall be capable of withstanding the required power without arcing for 220 5s. In addition, the 1 H RF homogeneity of the triple resonance probe head must be such that a continuous 810o pulse (2 X 360o + 90o) must retain at least 50% of the integrated magnetization relative to a single 90o pulse, using an aqueous solution containing 100 mM NaCl; 6) Disruption of 2H lock operation shall be minimized during application of gradient pulses. The peak-to-peak amplitude for the largest signal in the difference spectrum calculated from two one-transient spectra, one recorded 200 microseconds after a25G/cm 1-m s square gradient pulse and one recorded without the gradient pulse, shall be less than 10% from the corresponding peak in the spectrum. The phase difference between the two one-transient spectra shall be minimal; 7) The system shall be equipped with a variable temperature control unit capable of providing less that 0.02o C sample temperature variation per 1o C room temperature change. The sample temperature control, using the pulsed field gradient triple resonance 5-mm probe head must operate over a rang e of -10o C to 60o C (100o C is preferred) with setting and control being independent of room temperature; 8) The 1H sensitivity specifications for the triple resonance triple-axis pulsed field gradient 5 mm probe using Wilmad-535 sample tubes shall be: (I) ASTM 0.1% ethylbenzene 700:1; (ii) 0.5 mg sucrose/ml D2O 80:1; (iii) 0.5 mg sucrose/ml in 250 mM KCl in D2O 67:1; 9) The upgraded console shall provide at least four frequency channels (with five being preferred) with direct frequency synthesis on all channels together with the capability of producing different asynchronous or synchronous composite pulse decoupling and different shaped pulses on all of these channels simultaneously and independently. The system shall be completely broadband and ca pable of observing all nuclei up to 1H (protons). The composite pulse decoupling schemes shall be freely programmable by the user and include the option for pulse shaping of the individual elements of the composite pulse. All four (or five) channels shall have identical specifications at low rf power levels, except that only two channels shall require operation over the frequency range from 555 to 605 MHZ (for 19F and 1H), and a minimum of three channels shall operate over the range of frequencies from 30 -- 243 MHZ (with 15 -- 320 MHZ being preferable) for all other (i.e., X) nuclei; 10) The console electronics shall be capable of 0.25 degree phase resolution, 0.1 Hz frequency resolution (with 0.01 Hz being preferable) and a 90 dB attenuation range on all four (or five) channels. The rf phase shall vary by no more than 10 degrees over an attenuation range of 40 dB from full power. The settling time after a phase shift during a pulse sequence shall be minimal; 11) The pulse programming system shall permit i mplementation of user-developed pulse sequences and shall be capable of conducting all experiments published in the volumes 1 -- 3 of the Journal of Biomolecular NMR. It shall be possible to specify at least 30 independent pulse sequence interval lengths and 30 pulse widths in a single pulse program. The minimum interval length shall be no greater than 500 ns. It shall be possible to specify each interval length in increments of 25 ns or less. It shall be possible to write and execute pulse programs with at least 256 steps (without loops), with each step representing a time period during which any combination of pulses on the four channels is given. The amplitude and phases of the pulses shall be arbitrarily programmable, subject only to the resolution limits on the phase shifters and rf attenuators. It shall be possible to include at least twenty loops within a single pulse program, with independent loop counters. It shall be possible to nest loops; 12) The long term pulse amplitude stability on all ch annels shall be 1% and phase stability shall be better than 1 degree, as measured over a 24 hour period in a room where the temperature changes by less than 1.5o C. This phase stability is measured from the relative difference between 1D spectra, recorded with a 30 degree flip angle pulse, at various times during a 24 hour period; 13) The console electronics shall permit application of user defined shaped pulses to operate independently on each of the four (or five) available channels. The shaped pulses shall allow a minimum of 16000 user-definable elements within a single pulse shape. Waveform memory shall be at least 64K ram with 256K being preferred. The dynamic range of each channel for shaped pulses shall be at least 60 dB total range with 0.1 dBresolution at half range; 14) The system shall be capable of independent and simultaneous control over amplitude, frequency, phase and duration of pulses for all four (or five) frequency channels and over internal real-time clock pulses for triggering of e xternal devices; 15) Before high-power amplification, pulse rise and fall times shall be < 300 ns, measured between 10% and 90% amplitude levels. Fast power switching ( 4 us) shall be provided on all four (or five) channels; 16) The RF amplifiers shall be 100 Watt linear for 1H and 19F transmit pulses (at 550 -- 600 MHZ) and 300 Watts linear for all other transmit pulse amplifiers up to at least 243 MHZ for X nuclei. The 1H amplifier shall be capable of operating at 10 Watt CW and the X nucleus amplifier shall be capable of operating at 30 Watt CW. Operation of all transmit pulse amplifiers shall be under computer control. The RF amplifiers shall be capable of performing spin lock experiments on the 5-mm triple resonance gradient probe for up to 200 ms for 1H(gB1 = 12kHz) and up to 50 ms for the other channels (gB1 = 12kHz at 175 MHZ; gB1 = 4kHz at 60 MHZ) with droop 2%; 17) The upgraded console shall be equipped with a digitizer of at least 16 bits allowing simultaneous sampling of the quadrature receiv er channels using two digitizers and two sample and hold amplifiers for spectral widths of up to at least 150 kHz (200 kHz is preferred). The system shall be capable of oversampling (at least 2X) and should be capable of accepted industry standard digital and analog filtering of the NMR audio signal; 18) The console shall be equipped with a minimum 1280X1024 17 inch (19 inch is preferable) high resolution color monitor; 19) A minimum of 16 additional TTL lines that can be addressed by the pulse program for external device control shall be provided; 20) The dynamic range of the upgrade console shall be at least 60,000:1 as measured for a 90o 1H pulse by a S/N of at least 60:1 on a t-butanol peak in a 1/10,000 1H molar ratio to water; 21) The console shallbe equipped with ethernet TCP/IP capability. The host computer system shall operate under the UNIX operating system and provide standard UNIX utilities and a C compiler. The host computer shall contain a minimum of 128 M-byte of memory. The system shall i nclude a laser printer with software packages for plotting spectra. The system shall contain at least two serial ports, a keyboard and an industry standard mouse. The system shall include as a minimum a 6X CDROM drive. The vendor may propose in addition a quarter inch tape drive with 150 M-byte per cartridge (unformatted); 22) The system shall be equipped with two fast access disk systems, one containing at least 1G-byte of storage (unformatted) and one containing at least 4 G-byte of storage (unformatte d). Upon consultation with the vendor, one or more of the mass storage devices may be purchased separately by NHLBI and installed by the vendor who will assume responsibility for the entire system including the mass storage devices. The system shall includea 4 G-byte DAT tape drive; 23) The system shall be equipped with a SCSI interface (two are preferred) for control of up to at least 8 devices per SCSI controller; 24) The system shall have the capability of processing and analyzing data from a previous experiment while simultaneously acquiring data for a new experiment. This statement shall hold true for both one- and multi-dimensional experiments, up to four dimensions; 25) The transverse excitation profile for a G3 inversion pulse (Emsley and Bodenhausen, Chem. Phys. Lett., 165, 4 69 (1990)) of 3 ms duration shall be within a factor of two from the simulated value over a bandwidth of 1 4kHz; 26) The upgraded system including probes supplied new shall be covered under full hardware and software warranty for a period of a minimum of one year after all guaranteed specifications resulting from this contract have been met in the buyer's laboratory; 27) The vendor shall take full responsibility for the entire system, including console, computer and supplied peripherals, shim system and sup erconducting magnet. The vendor shall also warrant that all applicable specifications quoted in their published documentation will be met in the buyer's laboratory; 28) The acquired data shall be available as a file with equally spaced data points for ready off-line processing with standard software packages; 29) The peak-to-peak difference spectrum calculated from two spectra (four scans each) recorded under identical conditions, 30 minutes apart without removing the sample, shall be less than 2% of each individual spectrum; 30) The peak-to-peak spin echo difference signal for the anomeric proton in sucrose (two scans) shall be less than twice the intensity of the satellites for 10 consecutive experiments; 31) There shall be no sidebands or other spurious artifacts in the spectrum larger than 10% of the anomeric proton's satellite intensities. The signal-to-noise shall be larger than 20:1 for a provided sample containing 50 mg sucrose in 0.5 ml D2O. The spectra are to be recordedat 30o C unless otherwise indicated. 360 MHZ: 1) The upgraded console shall be capable of operating at or above 360 MHZ 1H (proton) frequency and in the range of at least 20 -- 200 MHZ (with 10 -- 243 MHZ being preferable) for X nuclei up to and including 31P. This upgraded console shall be interfaced with the existing 89 mm clear bore (wide bore) Oxford magnet, upper and lower shim stacks, and existing probes and related hardware or the necessary modifications, replacements or substitutions made (at the discretion and approval of the project o fficer) to this existing equipment in use such that the working spectrometer (console, probes, interfaces, magnet, computers and related hardware devices) is identical in all respects (except for age of hardware not actually replaced) to spectrometers currently being marketed by the manufacturer. The Contractor shall take full responsibility for the entire system, including probe heads, shim system and superconducting magnet. Note: Since 360 MHZ is not a widely available frequency, offerors may quote spe cifications for 300 MHZ and provide data at 300 MHZ although the delivered console shall be capable of observing proton resonances at 360 MHZ and using a deuterium lock; 2) The upgraded console shall be equipped with and use a minimum of 17 room temperature shim gradients for a wide bore magnet with a clear bore of 89mm designed for the highest magnetic field strength homogeneity. The upgraded console shall have the capability to perform computer controlled automated shimming of the magnetic field. Adjust ment of the superconducting magnetic field strength or shims required to obtain optimal room temperature specifications and shim performance shall be the responsibility of the Contractor and shall be carried out after consultation and in accord with the project officer; 3) The upgraded console shall have the capability to perform inverse detection NMR experiments for X frequencies in the range specified in 1 above; 4) The upgraded console shall include a power supply capable of generating simultaneously and independently power to drive three orthogonal gradients in three axis gradient probes. The shape, amplitude, duration and polarity of these gradients shall be under pulse program control and the use of various waveforms including sine shall be possible. Gradient amplifiers shall employ eddy current compensation and be linear, low noise, and preferably constant current. This system shall be capable of generating a field gradient along the z axis (axis of the magnetic field) with a strength of at least 25 G/cm on the 5-mm probe head (see next item). Gradients in the x and y dimensions of the three-axis probe shall be at least 25 G/cm. The offeror shall describe in detail in their proposal their strategy and procedure, including automation when applicable, for performing gradient shimming (magnetic field mapping). The offeror shall optimize the homogeneity of the region sampled by the 1H coil in e (below) including mapping of the field using gradient techniques on the existing 89 mm bore 360 MHZ Oxford ma gnet in the buyer's laboratory; 5) The system shall include a triple resonance 5-mm three-axis pulsed field gradient probe for observation of 1H while decoupling 13C and 15N, include 2H lock, and the 90o pulse widths must be < 10 5s for 1H for an aqueous non ionic sample, < 15 5s ( 12 5s is preferred) for 13C for an aqueous non ionic sample, and < 44 5s ( 35 5s is preferred) for 15N for an aqueous non ionic sample. The probe head shall be capable of withstanding the required power without arcing for 220 5 s. In addition, the 1H RF homogeneity of the triple resonance probe head shall be such that a continuous 810o pulse (2 X 360o + 90o) must retain at least 50% of the integrated magnetization relative to a single 90o pulse, using an aqueous solution containing 100 mM NaCl; 6) Disruption of 2H lock operation shall be minimized during application of gradient pulses. The peak-to-peak amplitude for the largest signal in the difference spectrum calculated from two one-transient spectra, one recorded 200 microseconds after a 25G/cm 1-ms square gradient pulse and one recorded without the gradient pulse, shall be less than 10% from the corresponding peak in the spectrum. The phase difference between the two one-transient spectra shall be minimal; 7) The system shall be equipped w ith a variable temperature control unit capable of providing less that 0.02o C sample temperature variation per 1o C room temperature change. The sample temperature control, using the pulsed field gradient triple resonance 5-mm probe head shall operate over a range of -10o C to 60o C (100o C is preferred) with setting and control being independent of room temperature; 8) The 1H sensitivity specifications for the triple resonance triple-axis pulsed field gradient 5 mm probe using Wilmad-535 sample tubes should be: (I) ASTM 0.1% ethylbenzene 300:1; (ii) 0.5 mg sucrose/ml D2O 30:1; (iii) 0.5 mg sucrose/ml in 250 mM KCl in D2O 20:1; 9) The upgraded console shall provide at least three frequency channels with direct frequency synthesis on all channels together with the capability of producing different asynchronous or synchronous composite pulse decoupling and different shaped pulses on all of these channels simultaneously and independently. The system shall be completely broadband and capable of observing all nuclei up to 1H (protons). The composite pulse decoupling schemes shall be freely programmable by the user and include the option for pulse shaping of the individual elements of the composite pulse. All three channels shall have identical specifications at low rf power levels, except that only two channels shall require operation over the frequency range from 333 to 365 MHZ (for 19F and 1H), and a minimum of three channels shall operate over the range of frequencies from 20 -- 200 MHZ (with 10 -- 243 MHZ being preferable) for all other (i.e., X) n uclei; 10) The console electronics shall be capable of 0.25 degree phase resolution, 0.1 Hz frequency resolution (with 0.01 Hz being preferable) and a 90 dB attenuation range on all four (or five) channels. The rf phase shall vary by no more than 10 degrees over an attenuation range of 40 dB from full power. The settling time after a phase shift during a pulse sequence shall be minimal; 11) The pulse programming system shall permit implementation of user-developed pulse sequences and shall be capable of c onducting all experiments published in the volumes 1 -- 3 of the Journal of Biomolecular NMR. It shall be possible to specify at least 30 independent pulse sequence inte (0176)

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