1. Field of the Invention
The invention concerns a device for performing chemical reactions and processes in high frequency fields.
It allows the advantageous introduction of energy and carrying out of disintegration, hydrolysis, chemical synthesis, extraction and drying as well as other reactions and processes under the effect of high frequency.
2. Description of the Related Art
For the running, acceleration and/or initiation of chemical reactions and processes an introduction of energy is often needed. For this purpose the reaction mixtures, are arranged, for example, in a microwave system with a radiation-screened housing in reaction containers that allow microwaves to pass through them, and energy is introduced through radiation with microwaves. Since with the reactions and processes that take place high pressures often result or the reactions only run under pressure, the entire arrangement must be stable under pressure and, for example, have a locking cover system. In general the reaction vessels are also fitted with safety or control devices, in order to be able to monitor the running of the chemical reactions and processes.
Equipment arrangements for the introduction of thermal energy in disintegration, hydrolysis, chemical synthesis, extraction, drying and other reactions and processes have been extensively described, but also have the likewise known disadvantages such as long heating and/or reaction times, limited or poor pressure and/or temperature stability and a lack of flexibility of the individual arrangements. Furthermore and as a rule, only reactions and processes in individual vessels, or a small number of parallel reactions, are possible. The stated disadvantages have in part been overcome by the use of high frequency energy to activate chemical reactions and processes, but here also there are limits on the number of sample vessels. Patent DE 43 25 667 A1 describes a device that allows the execution of six, eight or ten reactions simultaneously. Here the sample vessels with the samples are placed individually on a horizontal rotating table, secured to this, and moved on it in the plane of the table through the microwave field. This type of sample preparation requires, compared with the actual reaction time, long set-up times and in many cases involves a danger of misanalysis, since in particular because of the extensive time-consuming sample preparation the waiting times of the individual reaction mixtures can differ greatly. In these cases the assessment of the microwave radiation on the samples is only comparable to a limited extent and in practice can lead to not inconsiderable misinterpretations. The structural shape of the reactor system does not allow automated sample preparation that, with parallel syntheses in particular, leads to a large amount of time spent on sample preparation with high error rates. Genuinely high throughput screening is not possible with these reactor systems for the stated reasons.
In Tetrahedron Lett. 1998, 39, 1117-1120 the use of simple multi-corrugated plates in a domestic microwave unit is described. The use of these corrugated reactors for parallel synthesis in the microwave field is, however, associated with technical shortcomings such as a lack of pressure stability, low temperature stability of the reactor materials, poor energy distribution and associated variations in temperatures in the individual reactors as well as consistent temperature and concentration gradients in the individual reaction mixtures. It can be assumed that the stated weak points lead to a number of misconceptions during material screening.
The object of the invention is to fashion, with the least possible effort, a practical device with which a number of chemical reactions and processes in high frequency fields can be carried out under an improved and in each case extensively the same high frequency effect on the individual reactions and processes. In particular, misconceptions in material screening that can occur due to sample specifics such as temperature and concentration gradients, as well as shortcomings of the device and its application, should be avoided.
The invention envisages a magazine-type sample rotation body in the high frequency chamber arranged so that it rotates away from the horizontal, for the stacked, fixed-location accommodation of liquid- and gas-tight sealed or sealable, or single- or multiple, reaction blocks. These are pushed into the sample rotation body and with this are moved around their axis of rotation in a quasi xe2x80x9coverheadxe2x80x9d manner. Here the reactor blocks can each be stacked individually in the sample rotation body, or reactor blocks already existing in a stack are introduced and secured simultaneously. With the movement of the sample rotation body the individual samples are mixed in order to generate homogenous and comparable state conditions. Furthermore, the reactor blocks with the samples to be treated with the high frequency radiation and which have been mixed with the movement are transported through the radiation field(s) so that the radiation can have its influence with the same effect on each of the samples that can be present in quantity for simultaneous treatment. Any inconsistencies in the high frequency fields are thus extensively balanced out in terms of their effect on the radiation treatment of the sample in the multiple chemical reactions and processes. A device is fashioned that is loaded with the minimum of effort and in a short time and can be loaded with a number of reaction mixtures, equipped for high frequency treatment with comparable analytical conditions of the individual samples. Although a number of simultaneous sample reactions can be carried out, nevertheless at the start of and during the high frequency effect for the reaction mixtures essentially comparable sample and treatment conditions are guaranteed, so that misanalyses during material screening are extensively excluded. As a result in particular of the short apparatus set-up time (even for many samples, for example due to automatic sample preparation) during high frequency treatment and preparation for this, the analytical drawbacks of differing sample specifics such as temperature and concentration gradients, can to a large extent be avoided.
As a result of the advantageous low effort, fast and very practical loading, treatment and removal of a number of samples, the preconditions are created for genuinely high throughput screening.
For the reactor blocks preferably sample vessel plates can be used, which in the already known manner exist as corrugated analysis plates with sample vessels incorporated and arranged in a fixed grid or as sample carrier plates with sample vessel inserts. The latter can likewise have the known grid dimension of the sample vessels, so that connection with the advantageous so-called liquid handling technique is possible. The said high throughput screening is also supported by this.
Further advantageous structural designs of the characteristics of the independent claim are described and claimed herein. These concern, for example, the acceptance and the liquid-proof sealing of the reactor blocks with the sample vessels.