Nuclear Magnetic Resonance Spectrometer (600MHz)
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1 Nuclear Magnetic Resonance Spectrometer (600MHz) Specifications: State of the art analytical 600 MHz Nuclear Magnetic Resonance Spectrometer with Multi Nuclear Liquid and Solid CP-MAS Probes. I. Spectrometer Frequency: 600 MHz or better, optimum for general high field machine requirements with 2 Broad Band RF channels to run 2D NMR with various combinations of selected nuclei; having capabilities for the most up to date homo & heteronuclear multi-dimensional NMR experiments. II. Magnet specifications : Magnetic field: Tesla or better (a) 600 MHz NMR Spectrometer with Premium or Ultra Shield Plus or Selfshielded magnet Tesla, Shortest possible 5G (0.5mT) fringe field, shielding technology should be latest. (b) Anti Vibration Platform to damp the vibration of frequencies >3 Hz; Specify attenuation of critical frequency > 3 Hz. (c) State of the art room temperature shims as well as cryo shims for best line shape with line width, include all other related items (specify full details with technology) Configured to meet optimal probe line shape specification. (d) Field drift ( 6 Hz/hr), Radial Stray Field (0.5 mt line < 1.0 m), Axial Stray Field (0.5 mt line < 2.0 m) specify the actual values. (e) Helium hold time 150 days& Nitrogen hold time 14 days Specify:Evaporation rate/hr. and Refill volumes. (f) One liquid helium Transfer Line; Liquid Nitrogen Transfer Line. (g) Lock channel should be compatible with gradients and gradient shimming. (h) Special tool kit for magnet. (j) Helium and Nitrogen level measuring sensor system and corresponding automatic digital level meter displays. (k) At least 28 shims for obtaining optimum line-shapes with <7/14 Hz 1H line shape at 0.55% and 0.11% of peak height respectively on non-spinning chloroform sample.
2 III. Console and Electronics: (a) Advanced design two channel spectrometer capable of performing all single and multi-dimension experiments in all kind of samples including 90% H2O with 10% deuterated solvent; fast switching time for all parameters, without any hidden delays along with its importance in the quality of the spectra. It should include the capability of programming for modern pulse shaping, amplitude, phase and composite pulse decoupling sequences, preamplifiers with standard filters and digital receiver control with oversampling and with either digital quadrature detection with digitizer s facility for complete elimination of quadrature/ centre spikes or a direct digital receiver. (b) Linear amplifiers for 1 H and X nuclei with fast blanking and rise/fall times. (c) Modern communication system through fast Ethernet port to spectrometer. (d) Single Receiver with two hardware channels. KINDLY PROVIDE PRINTED SPECIFICATION SHEET Two identical independent RF channels system in addition to lock channel to handle nuclei such as 1 H, 13 C, 15 N, 19 F, 31 P, 11 B, 27 Al, 199 Hg, 51 V, etc. with high resolution in frequency, amplitude and phase. Mention switching times for all RF parameters. Frequency generation, digital receiver controls with over sampling and digital filters. High performance power transmitters for 2 channels (with provision for addition of 1 more in future). (f) Computerized Sample lift, eject/insert and spin control for liquid state. (g) High bandwidth receiver system with digital quadrature detection. Digital lock with high stability. Automated computerized lock control. 16 bits or more Analog to Digital Converter. (h) Auto Shim Facility. (i) Complete pulse shaping capabilities on both channels. (j) Special tool kit for spectrometer. (k) Digital quadrature receiver; Digital acquisition system providing <0.01 degrees phase resolution and <0.005 Hz frequency resolution. (l) Single Receiver with two hardware channels including digital filter and over sampling, digital filtering upto 5 MHz bandwidth with facility for automatic removal of quad-images and dc artifacts
3 (m) Transmitter system with transmitter power more than 100W pulse power for1h/19f and 500W for multinuclear work (6-640 MHz) (n) For solid experiments, transmitter with following transmitter power preferably of 1H ( 100 W) and X (500 W) and Variable temperature operation from 20(or lower)to +80 o C Gradient amplifier (a) Single axis gradient amplifier with gradient shimming facility with a gradient strength, specify the parameters. (b) High performance pulsed field gradients with gradient strength of 30G/cm or more on Z-axis with Gradient shimming. KINDLY PROVIDE PRINTED SPECIFICATION SHEET IV. Variable temperature accessories Low and high temp unit along with all accessories for control of sample temperature from -150 o C to o C with 0.1 o C accuracy. Temperature control unit with accessories for control of the temperature. KINDLY PROVIDE PRINTED SPECIFICATION SHEET V. Probes: 1. A Multinuclear 5 mm double resonance Broadband liquid Probe with Variable temperature facility to cover nuclei preferably 15N to 31P, and one channel capable of tuning for 1H and the other for X Nuclei with dedicated Lock channel and VT accessory for -100 C to +150 C. Automatic tuning and matching for all observation Nuclei. At least 200 numbers 5 mm NMR tubes along with 5 turbines and 200 numbers 3mm NMR tubes along with 5 suitable turbine to go in to 5 mm probe to run experiments with less amount of solvent should be provided along with the probe. Sensitivity: 1H 850:1.for % Ethyl Benzene sample 13C 360:1..for.10% Ethyl Benzeneor 330for ASTM sample 31P 150:1.for M TPP 15N 40:1.for.90% Formamide 19F 850:1 for.0.05% TFT
4 Line Shape and Resolution: 1H with CHCl3 sample Spinning 50% 0.6 Hz 0.55% 6.0 Hz 0.11% 12.0 Hz Sidebands 1% 13C with ASTM sample 50% 0.3 Hz 0.55% 4 Hz 0.11% 6.0 Hz Sidebands 1%(NT-4) Channel 90 o Pulse Width Sample 1H 11μsec 1% 13C-Iodomethane or 0.1% 13C-Methanol/99% D2O 13C 13μsec 1% 13C-Iodomethane or 0.1% 13C-Methanol/99% D2O 15N 25μsec 90% Formamide 31P 15μsec M TPP 19F 15μsec 0.05% TFT Gradient Strength: Maximum Z-gradient strength 30 G/cm Gradient recovery time* 100 us (95% signal amplitude) * With sample 0.1 mg GdCl3 / ml D2O + 1% H2O + 0.1% CH3OH; 5 ms gradient square pulses with strength +/ 37.5 G/cm KINDLY PROVIDE PRINTED SPECIFICATION SHEET. 2. Solid State CP MAS Probe 3.2mm rotor with fast MAS 20KHz spinning speed to cover nuclei in the range of 15N to 31P, Frequency range: 60 MHz to 242.9MHz (X channel)and 1H/19F observe and decouple as well as Variable temperature accessory to perform experiments at various temperatures in the range -20 C (optionally lower temperature down to 10K) to +80 C. At least 25 rotors should be included with the probe of Zirconia (15Nos.), Silicon Nitride(10 Nos.) with appropriate caps. Possibility of combined rotation and multiple-pulse spectroscopy (CRAMPS) experiments. List number of pulse sequences available in ready to use mode.
5 Sensitivity: 13C 250:1 in double (HX) resonance mode Resolution:0.1 ppm or better for Adamantane (13C) KINDLY PROVIDE PRINTED SPECIFICATION SHEET. 3. One 3mm/5mm Probe with gradient facility covering Nuclei range 15N to 31P for X channel and 1H, 19F for Hi band with Variable temperature accessory for -100 C to +150 C range. KINDLY PROVIDE PRINTED SPECIFICATION SHEET. VI. VII. Autosampler: Fully functional, compatible, for 60 or more samples with auto-inject mode and spinners. Data System: (a) Hardware: PC with suitable latest operating system with latest upgraded software for 1D, 2D,3D & 4D acquisition and processing. (i) Two Desktop computers, one for data processing and another for operation of NMR instrument with minimum Pentium i7 Quad or higher processor, DVD-RW drive facility, 500GB HDD, >16GB DDR RAM, 24 inch LCD Monitor, Minimum 4 USB ports and two Ethernet ports for data acquisition and internet. ii) 10 additional software license for offline data processing from Satellite Workstation. iii) One additional Latest Laptop suitable to run NMR data Processing software. iv) Printer: Suitable Color laser printer. (b) Software: Most comprehensive latest NMR software capable of all up-to-date heteronuclear multi-dimensional NMR experiments including latest experiments for reconstruction of multi-dimensional NMR spectra. Package should include all the latest pulse sequences for multi-dimensional NMR experiments available with the vendor. Please provide list of pulse sequences available for ready use. Specific software to have non-uniform data sampling and processing to facilitate 10 % data acquisition for linear prediction. Licensed Software Modules should include the following: Acquisition, Processing, Plotting, Multiplet Analysis, Deconvolution, Automation,
6 Projection Reconstruction Spectroscopy with networked laser jet color printer. Any software upgrade (pulse sequence and processing) or new software (pulse sequence and processing) that are released during the warranty periods should be given to the user free of cost. Software should be provided in CDs. VIII Vendors are required to arrange for all the cryogenics including liquid Helium/liquid Nitrogen and related accessories required for charging and installation of the magnet as well as Low Temperature probe, if any. IX. UPS system: Appropriate standard make UPS (and isolation transformer) with at least one hour back up for the uninterrupted and smooth functioning of the entire system. The rate should be quoted in Indian rupees. The power requirement for proper functioning of the NMR spectrometer along with all accessories should also be provided by the vendor. X. Consumable Accessories (i) Standard samples kit of NMR System for Acceptance test procedure. (ii) Line shape sample and sensitivity samples for 1H, 13C, 15N, 19F, 31P. (iii) NMR tubes 5mm-200 nos. 3mm-200 nos. (iv) Spinners for low and high temperature applications (10 numbers-5 for 3mm and 5 for 5mm tubes). (v) 3.2mm rotors, Zirconia (15Nos.), Silicon Nitride (10 Nos.) with appropriate caps. (vi) Liquid nitrogen transfer tube (10meters). (vii) Liquid Helium Transfer line. (viii) Special tool kit for magnet/spectrometer. XI. XII. Warranty: Five years on-site comprehensive warranty including maintenance. The warranty should include all parts of NMR spectrometer and its accessories. Service: Service problems should be attended within 72 working hours. In case of breakdown during the warranty period, a competent service engineer of the
7 supplier should make as many visits as are necessary to rectify the problem and replace the faulty parts. XIII. XIV. XV. Quote must have a compliance report on all the above points. A detailed specification sheet highlighting all above specification along with detailed experimental conditions must be attached. Operation and Service manuals (in English) with schematic diagrams should be provided. Training: Training on applications for two persons for at least one week should be provided at factory and Training for 1 week onsite. XVI. XVII. Delivery Time Specify delivery time for the machine from the date of opening LC. The following technical requirements should be strictly met and necessary document has to be enclosed along with the main quotation. (i) Maintenance network : Mention address of the institutions where the systems are in working conditions. Mention the maintenance network in India for the instrument. (ii) Policy against magnet quench (iii) Initial helium fill for charging the magnet to be provided by the vendor. (iv) The spectrometer and its components must be OQ, PQ & IQ 1 compliant. (v) The vendor should have installed 600MHz NMR machine in India and a documentary evidence of the same and evidence of satisfactory working & after sale support to be submitted along with tender document. (vi) Availability of applications/service Engineer to handle instrument problems immediately. (vii) All manuals (service & operational) should be given as hard copies and/or soft copies on CDs. (viii) Complete product catalogues describing all the required basic items should be produced. (ix) If required, vendor should be able to give demonstrations about the capabilities of the spectrometer and all the components at Indian sites. (x) Please quote price of each item separately in separate sheet.
8 (xi) Upgradation of software should be given free of cost as and when the new extension versions are released by the manufacturer/vender at no additional cost during the period of warranty. (xii) Price for the installation charges should be quoted separately, if any. (xiii) In case of magnet quench during the installation or at subsequent times due to faulty design, the necessary costs for recharging or replacing of magnet should be borne by the vendor. XVIII. Scroll Compressor should be included with the system to supply compressed air to the NMR system along with suitable Air drier and storage tank of 500 litres capacity. XIX. Incomplete tender documents without compliance statements will be rejected without assigning any reason.
9 OPTIONAL (to be quoted separately in separate sheet) 1. Softwares Softwares for Structure Verification, Structure Prediction, Experiment Simu - lation, Spectra Simulation, Teaching Software, Protein dynamics analysis for the 600MHz NMR Spectrometer. 2. Upgradation/Refurbishment of existing Varian 400MHz NMR Spectrometer as per the following specifications: Latest Version of electronic console with Full Band 2-RF CHANNELS: Capabilities of 1H/19F observe and decoupling with X nuclei. With best frequency and phase resolution, fast switching time for all parameters, without any hidden delays. It should include wave form generators for pulse shaping, amplitude, phase and composite pulse decoupling generator, preamplifiers with standard filters and digital receiver control with oversampling and quadrature detection with digitizers facility for complete elimination of quadrature spikes. 2-Channel Amplifier System: High Band (1H /19F) amplifier minimum 50 W and Low band (or Broad) band (X) amplifier minimum 150 W. Variable Temperature Controller, at least in the range of -100C to +150 C, with Low- and high-temperature accessories. 5mm multinuclear Broad Band Direct/observe Z gradient Probe capable of covering nuclei range 1H, 19F, 31P to 15N, 39K, 109Ag with computer controlled automatic tuning and matching (ATM) and able to perform all the inverse experiments with high S/N ratio for 1H in 0.1% Ethylbenzene of 450 or more,13c in 10% Ethylbenzene in with 210 or more, 19F with 500 or more, 31P with 100 or more and 15N with 30 or more on standard test samples. Latest NMR acquisition and Processing software with Plotting, Structure Verification and Analysis-1D and 2D (HSQC, TOCSY, COSY, HETCOR, NOESY, HMBC, DOSY etc.), Multiplet Analysis, Deconvolution, Automation, Projection Reconstruction Spectroscopy. Software: The software should be latest one and should function all latest parameters in automatically. PC controlled Windows based operating system for NMR Data acquisition and processing of 1D, 2D, 3D and 4D experiments.
10 The vendor should provide twenty floating licenses along with one processing PC (with latest configuration) for off-line processing (Processing, Plotting, Structure Verification, Multiplet Analysis, Deconvolution, Automation, and Projection Reconstruction Spectroscopy). A complete set of operational manuals should be provided. List of accessories required: 1) Computer: A suitable Computer for Performing NMR operation should be provided. 2) Color laser printer. 3) Required Consumables and Spares: Consumables along with the machine such as spares, tool kits essential for routine operations. 100 liquid sample tubes with caps. 4) Other Accessories: Other equipment such as, Air compressor with sound- Proof casings, driers/filters, pressure gauge, necessary tubings, other cables required for connecting the machine to the control panel and so forth has to be supplied by the vendor. The required UPS with adequate power-backup with necessary connectors has to be provided by vendor/supplier along with the main NMR spectrometer. 5) Two 55 liter Dewars for the transfer of liquid nitrogen with pressure gauge and the required tubing of adequate length has to be supplied along with the machine. Warranty: Comprehensive on-site warranty for 1 year after completion of Standard one year warranty including all parts and labor. Free maintenance and service, regular upgrades to all software during entire warranty period. Equipment Qualification (IQ/OQ/PQ& DQ) Definitions: There are three types of protocol that are used to validate instrument performance satisfies regulatory requirements. IQ which refers to Instrument qualification is the pre-installation detail that the equipment, its component parts and location, are fit for the purpose and satisfy the objectives of the user to carry out the intended function to expected standards.the IQ qualifies the equipment is installed correctly with
11 tubing, fittings, syringes and valves connected appropriately. This Pre-qualification checks that all appropriate consumables relative to the agreed use, manufacturer s documentation, conformity and calibration detail is present. Upon delivery the engineer will: 4. Confirm all components are delivered as ordered. 5. Review hazard and safety precautions for area of use including materials that may come into contact with the instrument and personnel 6. Install hardware including all tubing s, syringes and valves. 7. Configure and install program application functions. 8. Conduct leak test. OQ which refers to Operations Qualification carried out by the manufacturer or supplier at installation or service interval to verify the performance criteria presented by the manufacturer, to confirm the instrument satisfies its agreed metrics, is valid in the working environment by verification against traceable references. The engineer will: Assure the system is functioning to acceptable limits by testing relevant instrument specification parameters and ranges as determined by Microlab Technologies Instrument Performance Validation protocol. At the completion of the OQ all of the operational tests are documented, results validated, all relevant certificates completed and signed. Once completed the engineer will provide instrument familiarisation training to confirm you are ready to run the instrument with confidence The scheduling of service and calibration intervals which are then diarised automatically to assure testing at next interval PQ refers to the test or validation protocol carried out by the user, offering documentary evidence that the instrument is maintaining the agreed values. DQ or Document Qualification should comprehensively describe:
12 The complete maintenance history, system history and inventory of components and documentation. Verification of components installation. Performance verification of laboratory equipment for routine R&D, QA/QC, EPA, FDA and client compliance. x
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