The subject matter of the contract includes the configuration, delivery and commissioning of an NMR spectrometer in the form of a benchtop instrument. The NMR spectrometer will be used for
- routine chemical structure elucidation and substance analysis
- online reaction monitoring and general synthesis monitoring
- Presentation of release processes (release kinetics) and quantitative drug analysis
- determination of the degree of substitution after chemical modification of polymers,
- Determination of the composition and distribution of the monomer units of copolymers (sequence analysis)
- Determination of molecular weight of polymers
- quantitative determination of the residual monomerge content of polymerization mixtures
- Monitoring and tracking of biodegradation of degradable components/substances
and be equipped and suitable for these applications.
The NMR spectrometer should be used in the chemical laboratory at normal room temperature between 18 and 28 °C. There it is to be used flexibly at variable locations. Exclusion criteria are therefore a required air conditioning of the device, the connection or required cryogenic cooling media and the connection to compressed air or shielding gas. The power supply of the device must be via a supply line with a protective contact plug customary in Germany at alternating voltage 230 volts with a frequency of 50 Hertz.
The NMR spectrometer must be easy to transport to different locations without great technical effort. Therefore, the NMR desktop device should only consist of a single housing (plus PC/laptop should be included in the package). The weight of the device may not exceed 75 kg, so that it can be easily carried by 2 people, lifted and positioned on a table and moved on a transport trolley for easy transport. For use directly in the fume cupboard, the device must not exceed the dimensions: 60 x 45 x 45 cm (length x width x height). It must later be optionally equipped with an automatic sample changer for up to 20 samples.
The device will be equipped with an NMR system that allows analyses on 1H, 19F, 13C, 31P, 7Li and 29Na with standard 5 mm NMR tubes. Preferably, the cores in the NMR device are only changed via the software, so that no manual adjustment (tuning / matching) on the spectrometer is necessary. In addition, the device should have an external fast hardware lock system, so that deuterated solvents are not needed to lure the NMR system.
The NMR resonance frequency should be at least 80 MHz for protons.
With a required resolution of
- Linienbreite < 0.25 Hz and 50 % Peakhöhe
- linewidth < 10 Hz at 0,55 % peak height, and
- Linienbreite < 20 Hz and 0.11 % Peakhöhe
a signal-to-noise ratio of a 1H single scan for 1% ethylbenzene according to ASTM Method E386−90 (Determination of the Sensitivity of NMR Instruments) of at least > 200:1 should be achieved.
For the application of flow NMR methods such as online reaction monitoring or general synthesis monitoring, the device is required to be equipped with a straight flow cell with minimal dead volume. The necessary equipment for carrying out flow NMR and for connecting the NMR device to the synthesis apparatus should be part of the package. When operating in Flow NMR, a signal-to-noise ratio equivalent to that of using the standard 5 mm NMR tubes is expected.
In addition to the hardware equipment of the device for NMR flow, a software-based effective solvent suppression forms the basis for sensitive online reaction monitoring and a high resolution of the NMR spectra, so that qualitative and quantitative determinations can be carried out in protonated solvents such as water with high sensitivity and the use of expensive, deuterated solvents is not necessarily necessary for NMR measurements.
The requirements for the individual process parameters must be found in the specifications including the appendix "Award conditions".