WO2004081560A1

WO2004081560A1 - Automatic analysis device for detecting agents in substance mixtures

Info

Publication number: WO2004081560A1
Application number: PCT/DE2004/000402
Authority: WO
Inventors: Robert Bischoff; Peter Ködderitzsch
Original assignee: Sensobi Sensoren Gmbh
Priority date: 2003-03-10
Filing date: 2004-03-03
Publication date: 2004-09-23
Also published as: DE20303748U1

Abstract

The invention relates to a system for carrying out the automatic qualitative and quantitative analysis of substance mixtures which makes it possible to obtain analytical results comparable with the results of chromatography devices. Said system in its whole is embodied in the form of a simple and low-cost structure which can be used in an unfavourable environment. The inventive automatic analysis device consists of a pump in the form of an excipient microdosage unit (1), a sample supplying system (5) comprising a return valve which is embodied in the form of a six-port valve and provided with a sample loop, a sample injector, a detector and an evaluation system. Said microdosage unit (1), the sample supplying system (5), the sample injector in the form of a detecting module (8) and the evaluating system in the form of a data processing module (10) are embodied in the form of individual closed modules (1, 5, 6, 8, 10) which are provided with external electrically controlled connections and initiate electric signals.

Description

AUTOMATIC ANALYSIS APPARATUS FOR THE DETECTION OF AGENTS IN STOFFGEMISC _HE N

The invention relates to an automatic analysis apparatus for the detection of agents in substance mixtures.

For qualitative and quantitative analysis of mixtures of substances, automatically working analysis devices are used, which are based on chromatographic methods. One of these methods is high-resolution liquid chromatography (HPLC). For this purpose, a number of HPLC machines are known from the general prior art, the main components of which are usually a pump for an eluent, a sample application system with a switching valve with a sample / metering loop, and a sample injector, separation column and detector with evaluation system. Due to the sensitivity and complexity of the analysis equipment, these devices are generally only operated in laboratories.

For example, in the publication DE 39 43 524 C2, such a liquid chromatograph with a column for separating a sample, an input part for feeding a mobile phase to the column, a sample input part for taking the sample from a sample needle into a sample loop, a channel switching valve, a Detector part described as essential parts. The special feature is that in a "through position" there is a direct connection through a container of the mobile phase to the drain opening and the pump is operated at high speed to replace the mobile phase.

Further special details can be found, inter alia, in the publication DE 196 41 210 AI, which discloses an apparatus and method based on HPLC for the separation of highly complex substance mixtures. Several separation column systems are combined with one another in order to carry out a coarse and fine separation and in the meantime separated fractional ready to be saved on fixed phases, which are later analyzed in a detector unit.

An HPLC analysis device is also described in the publication DE 199 26 163 AI, which is also constructed in the usual way, a vessel carrier with a mixing vessel, in which the sample containing a reagent is located, being subjected to a shaking motion before it is introduced.

The basic structure of the analysis apparatus corresponds in both cases to that of a conventional HPLC machine, which is used in laboratory operation and is costly.

The object of the invention is to develop an arrangement for the automatic, qualitative and quantitative analysis of mixtures of substances which enables analysis results comparable with chromatography devices, but in its entirety does not have such a complex structure which can also be used under unfavorable environmental conditions and can be produced economically ,

The object is achieved by the features listed in claim 1. Preferred further developments result from the subclaims.

An arrangement according to the invention for the automatic qualitative and quantitative analysis of substance mixtures of soluble solid, liquid and gaseous substances in the form of an analysis apparatus essentially comprises a microdosing unit with associated control device, the microdosing unit being based on an arrangement of three electrically controllable valves on a valve block; a sample application system consisting of four electrically controllable valves on a valve block as a sixport valve with a sample loop; a sample injection device; a detector module with an array of electrically conductive Sensors in a sample chamber as well as a data storage unit, an analysis control unit and optionally a data processing unit in the form of a computer as an evaluation system and control device for the analysis process, which are connected to one another and are operatively connected to one another.

The detector module consists of a sandwich-like arrangement of two supports for sensors, with an array, at least on one support, of electrically conductive sensors sensitive to different detergents, between which, for example, a film with a recess in the outer dimensions of the two supports, largely corresponding to the outer dimensions of the two supports Area of the sensors is arranged, the recess of which forms the gas and liquid-tight sample channel. This version of the detector module basically represents a multilayer arrangement, the intermediate layer for connecting the two layers by means of a cutout forms the sample channel with sensors arranged therein as an array, the channels opening into these for the passage of a sample, and connections of the electrically conductive sensors leading to the outside having. The values determined with the detector module in the form of electrical variables initiated by the sensors can be processed online as well as stored in a special memory unit, with subsequent processing and evaluation being possible.

Optionally, a separation column customary for the chromatography method can additionally be arranged between the sample application system and the detector module.

The advantages of the invention consist in particular in its robust and low-mass construction. All pumping processes required for the analysis process, including sample injection, are carried out by electrically valves with low energy consumption without the usual, complex mechanisms.

By using electrically conductive sensors to detect the agents contained in the substance mixture to be examined, only electrical signals can be evaluated, which reduces the susceptibility to faults. The analysis apparatus can be constructed in a modular manner, the microdosing unit with associated control device, the sample application system and the analysis module being designed as separate structural units which are only connected to one another for the on-site analysis. The analysis module can also have an implemented evaluation unit and / or data memory. The analysis apparatus can be made up of modules or as a closed unit with its own energy supply and can also be used unattended for long-term analyzes under difficult environmental conditions, such as under water or a toxic atmosphere, over long periods of time. The analytical apparatus, which has a wide range of uses, is, in contrast to the chromatographic apparatuses and devices in use to date, much more manageable and cost-effective.

The invention is illustrated as an exemplary embodiment with reference to FIG. 1 as a basic illustration of the arrangement for an automatic analysis apparatus

2 as a basic illustration of an analysis apparatus for monitoring analyzes and FIG. 3 as a basic illustration of an analysis apparatus for analyzing individual samples.

According to Fig. 1, an automatic analysis apparatus consists of individual, closed, external modules having modules. A microdosing unit 1 with associated control device 2 forms a first module, which is connected by means of conventional capillary tubes 3 to a source 4 for a carrier medium and a sample application system 5 as a second module, the sample application system 5 in turn having an injection module 6, a waste container 7 and one Detector module 8 is connected, which in turn has a connection to the waste container 7. The microdosing unit 1 is based on an arrangement of three electrically controllable valves, in particular solenoid valves on a valve block.

The control device 2 for the solenoid valves is by means of a control bus 9 as well as the second module with the sample application system 5, which consists of four electrically controllable valves, in particular bistable two-way solenoid valves on a valve block as a six-port valve with a sample loop, and the injection module 6, which is based on a modified arrangement of solenoid valves on a valve block for the microdosing unit 1 with an integrated control device 2, is connected to a data processing module 10, in particular in the form of a computer, via corresponding interfaces. The data processing module 10, which is also connected by means of a data bus 11 to the detector module 8, which is formed from a sample chamber with an array of electrically conductive sensors arranged therein, controls the interaction of the individual modules 1 by means of stored software; 5; 6; 8 and 10, thus the entire sequence of the analysis process and evaluates the signals of the detector module 8, the result of which is interpreted and stored, and can also be shown on a display and output as a hard copy. To fill the analysis apparatus, the microdosing unit 1 sucks in the carrier medium from the source 4, conveys it in excess via the sixport valve in the sample application system 5 for rinsing the detector module 8 to the waste container 7, while in parallel the injection module 6 inputs an excess sample into the sample loop at the sixport valve of the sample application system 5.

The excess is passed into the waste container 7. The bistable two-way valves of the six-port valve are switched by means of a control signal from the data processing module 10, so that the sample loop lies in the flow of the carrier medium and the sample is fed to the sample chamber in the detector module 8 by the pressure of the carrier medium. The signals initiated in the array of electrically conductive sensors are transmitted to the data processing module 10 and further processed by the latter.

In an alternative variant (not shown), a microprocessor with a stored control program and a memory for analysis data and values can be implemented in the detector module 8 to control the analysis process, the detector module 8 using the control bus 9, which is then connected to it, with the Microdosing unit 1, the sample application system 5 and the injection module 6 is directly connected. Furthermore, it is favorable to implement the injection module 6 in the module of the sample application system 5. An analytical apparatus assembled in this way can be used over a long period of time with its own energy supply as an autonomous system for collecting values from a series of analyzes, reconnected to the control and data processing unit, the values and data read from the memory and further processed with external data processing modules 10 , In this context, it is also conceivable to wirelessly transmit the values and data stored in the memory to a receiver for forwarding to a data processing module 10 by means of a transmitter likewise integrated in the detector module 8. A separation column customary for chromatography processes can also be arranged between the sample application system 5 and the detector module 8. The process of analyzing a substance Mixtures are then carried out in an analogous manner to conventional chromatography devices.

In addition to the capillary tubes 3, which serve to transport the carrier medium and the medium of the sample, only electrical connections to or between the modules are required, since these are controlled by means of electrical signals, feedback and measured values or data are also available as electrical quantities. In a variant, the automatic analysis apparatus, which can be used in particular for analyzes to monitor the quality or composition and deviations from predetermined values of an analyte, can in the simplest case consist of the detector module 8 and the sample application system 5, the detector module 8 being over An integrated analysis sequence control and data memory for measured values can have an interface (not shown) with peripheral devices for analysis control and evaluation of the measured values of the electrically conductive sensors in the sample chamber of the detector module 8 and can be connected via the control bus 9 to the sample application system 5. The analyte is fed to the detector module 8 via a capillary tube 3 from the sample application system 5. By means of a pump 12, an analyte is continuously taken, for example from a body of water 13, which flows through the sample loop under pressure in the "filling" position of the sixport valve in the sample application system 5. The sixport valve is switched to the "inject" position in a predetermined manner Intervals so that the chemical composition of the analyte is examined at regular intervals and changes are registered, and the data is used to control and regulate subsequent processes or to issue warning messages. In an analogous manner, the analysis apparatus consisting of the detector module 8 and the sample application system 5 can be used for transferring monitoring of the composition of media in pipelines can be used by connecting the sample loop as a bypass to a transport system of an analyte. The automatic analysis apparatus according to FIG. 3 basically has the same structure as that shown in FIG. 2, but is preferably used for examining individual samples or batches of samples. In the course of the analysis of a sample which is located in a sample container 14, the pump 12, the conveying direction of which can be switched over and which can be a microdosing unit 1, in a first essential step conveys a carrier medium from the source 4 for rinsing the sample application system 5 via an outlet into the waste container 7. In the second essential step, the conveying direction of the pump 12 is reversed, at the same time the outlet of the sample application system 5 is connected to the sample container 14, whereby the analyte is sucked out of the sample container 14 into the sample application system 5 and fills the sample loop. In the third essential step, the direction of delivery of the pump 14 is reversed again at a point in time at which the sample loop is safely filled with the analyte, but this has not yet flowed to the pump 12, the six-port valve in the sample application system 5 being switched over at the same time that the analyte from the sample loop is passed in a known manner through the sample chamber with the electrically conductive sensors in the detector module 8 by means of the pressure of the carrier medium. The signals initiated by the electrically conductive sensors are then treated in an analogous manner to that described in the example of FIGS. 1 and 2. Reference symbols used

1 microdosing unit

2 control device

3 capillary tubes

4 source

5 sample application system

6 Injection module

7 waste container

8 detector module

9 control bus

10 data processing module

11 data bus

12 pump

13 bodies of water

14 sample containers

Claims

claims

1. Automatic analysis apparatus for the detection of agents in mixed substances, characterized in that the analysis apparatus consists of a pump in the form of a micro-metering unit (1) for a carrier medium, a sample application system (5) with a changeover valve in the form of a six-port valve with a sample loop, and a sample injector , a detector and an evaluation system, the microdosing unit (1), the sample application system (5), the sample injector in the form of an injection module (6), the detector in the form of a detector module (8) and the evaluation system in the form of a data processing module ( 10) are designed as individual, closed, external connections having electrically controllable and electrical signals initiating modules (1; 5; 6; 8; 10).

2. Automatic analysis apparatus according to claim 1, characterized in that the automatic analysis apparatus consists only of a detector module (8) and a sample application system (5).

3. Automatic analysis apparatus according to claim 1 or 2, characterized in that a chromatographic separation column is arranged between the sample application system (5) and the detector module (8).

4. Automatic analysis apparatus according to claims 1 and 3, characterized in that the microdosing unit (1) as a module consists of an arrangement of three electrically controllable valves on a valve block with associated control device (2).

5. Automatic analysis apparatus according to claims 1 or 2, 3 and 4, characterized in that the sample application system (5) as a module consists of four electrically controllable valves on a valve block as a six-port valve with a sample loop.

6. Automatic analysis apparatus according to claims 1 and 3 to 5, characterized in that an injection module (6) consists of an arrangement of three electrically controllable valves on a valve block with an associated control device.

i

7. Automatic analysis apparatus according to claims 1 or

2 and 3 to 6, characterized in that a detector module (8) has a sample chamber with an array of electrically conductive sensors, the gas and liquid-tight sample chamber consisting of a multi-layer arrangement of two carriers with sensors with an intermediate, in the region of Sensors has a section as an intermediate layer having a sample channel and two channels to the sample channel.

8. Automatic analysis apparatus according to claims 1 and

3 to 7, characterized in that the evaluation system consists of a data processing module (10) with implemented software for controlling the interaction of the modules (1; 5; 6; 8; 10) during the analysis process.

9. Automatic analysis apparatus according to claims 1 or 2 and 3 to 6, characterized in that a microprocessor with a stored control program and a memory for analysis data and values are implemented in the detector module (8) for controlling the analysis process.

10. Automatic analysis apparatus according to claims 1 or 2 and 3 to 7 and 9, characterized in that a transmitter for transmitting the values and data stored in the memory to the data processing module (10) is integrated in the detector module (8).

HERE TWO SIDED DRAWINGS