Device for automatised sample handling

Abstract

An analytical system (10) comprises an analytical instrument (5) and a sample handling device (1). The sample handling device comprises an enclosure (2) for receiving at least one closed sample container, and an opening unit (3) for opening the at least one closed sample container. The opening unit (3) and the enclosure (2) are located in the immediate proximity of the analytical instrument (5).

Description

[0001] Device for automatised sample handling

[0002] The invention refers to an analytical system and to a method for automatised sample handling using an analytical system.

[0003] Analytical systems arranged for automatised sample handling are commonly used in laboratories to facilitate sample handling and to efficiently process large quantities of samples at one time. These can be used for handling samples to be analysed by an analytical instrument for trace elemental analysis, like inductively coupled plasma optical emission spectroscopy (ICP OES) or inductively coupled plasma mass spectrometry (ICP MS). A high degree of automation in sample processing has several advantages: it is faster and more efficient than manual processing and human operating errors can be minimised. Laboratory staff can meanwhile devote time saved to other tasks.

[0004] US 2022 390 477 A1 and WO 2022 026 265 A1 show autosampler systems for automatised sample handling comprising a sample cap remover that is integrated in the autosampler system to automatise and speed up decapping of the sample containers.

[0005] In nearly all of the common devices for automatised sample handling used in trace elemental analysis, for example, sample containers are open during the whole process of handling and analysing. Sample containers that are open for a longer time bear an increased risk of contamination of the sample, for example by dust particles in the ambient air or by crosscontamination between several open samples in the analytical system. The sample itself may also change its concentration by evaporation of the solvent. With an increased number of samples to be handled, the time during which the sample containers are open also increases, as they are all provided in an opened state at once and then handled one after the other. Risk of change in sample composition can then increase over time from sample to sample. Additionally, the evaporation of acids or organic solvents may impact the health of the lab personnel, be detrimental to the instruments in the lab and may, in the case of organic solvents, be a potential fire or explosion hazard.

[0006] Therefore, these types of analytical systems arranged for automatised sample handling are typically not used for high-risk samples or precise measurements, for example for semiconductor applications. Samples of this kind are often handled manually to avoid contamination. Alternatively, the whole autosampler with the open sample vials is put into a pure environment, with a filtered air flow around the sample vials. However, manual handling also has several disadvantages, such as an increased risk of mix-ups or inaccuracies. It also takes longer than automated handling and is therefore inefficient compared to automatised sample handling. Using autosamplers with a laminar flow of filtered air is costly, requires a lot of space, does only mitigate and not eliminate the problems mentioned above, while it often even increases the rate of evaporation with all related problems related.

[0007] The invention addresses the problem that during the time a sample container is open before it is used by the analytical instrument, the sample is vulnerable to contamination or alteration of the sample composition.

[0008] According to a first aspect the invention, the problem is solved by an analytical system which comprises an analytical instrument and a sample handling device. The sample handling device comprises an enclosure for receiving at least one closed sample container, and an opening unit for opening the at least one closed sample container. The opening unit and / or the enclosure is located in the immediate proximity of the analytical instrument. The enclosure is advantageously configured to be closeable to outside of (that is, external) the sample handling device (from where the at least one closed sample container is received). Optionally, the enclosure is configured to be further closeable to a remainder of the sample handling device or to at least the opening unit. The enclosure may be configured to be closed to the analytical instrument external the enclosure (the enclosure may be within the analytical instrument in some embodiments). In embodiments, the enclosure is sealable (when closed). These implementations may all reduce potential contamination of the sample.

[0009] The at least one closed sample container is usually provided in a sample rack that is designed to hold multiple closed sample containers. The enclosure is designed to hold at least one closed sample container. Preferably, it has a rack or similar structure to provide a secure support for the at least one closed sample container. It is also possible that several closed sample containers can be held by the enclosure at the same time. This can be preselected depending on the type of sample to be handled by the device and can help to save time. The opening unit, which may be designed as a decapper, such as a screw decapper depending on the type of lid or cap to be removed from the at least one closed sample container, serves to open the closed sample container. This step must be carried out in order to extract a sample from the at least one closed sample container and transfer it to the analytical instrument. To ensure that the safety risk is minimised, the sample should be opened as late as possible and as close to the analytical instrument as possible. Therefore, at least one and preferably both of the opening unit and the enclosure are located in the immediate proximity of the analytical instrument. Immediate proximity in this context means that the opening unit and / or the enclosure is either located in the analytical instrument or immediately adjacent to it, preferably less than 50 cm apart from the analytical instrument, particularly preferred less than 25 cm, more particularly preferred less than 10 cm.

[0010] It is possible to locate the opening unit inside the enclosure to minimise the transfer distance. The closer the enclosure is to the analytical instrument, the shorter the distance the sample must travel from the enclosure to the analytical instrument. This also shortens the time that the sample must be decapped (that is, open), thus minimising the safety risk, especially with hazardous substances or samples that evaporate quickly. The opening unit may also serve to close the at least one closed sample container after the sample has been taken from it. The analytical instrument may, for example, be an instrument for inductively coupled plasma optical emission spectroscopy (ICP OES) or inductively coupled plasma mass spectrometry (ICP MS), but also another suitable analytical instrument, such as a mass spectrometer having another type of ion source, for example an electron ionisation source.

[0011] According to an embodiment of the invention the analytical system further comprises a bar code reader. As a safety measure, the bar code reader can help to reliably identify the sample if the at least one closed sample container has a bar code so that mix-ups can be avoided. It also allows results gained in the analytical instrument to be assigned more quickly and automatically. It is also possible that the bar code reader is suitable for reading other identification features attached to the at least one closed sample container, such as QR codes or other matrix bar codes.

[0012] According to a further embodiment the analytical system further comprises a liquid dosing device. The at least one closed sample container can then be positioned below this device for adding, for example, an internal standard and / or a dilution fluid to the sample. In this way, the sample can be optimally prepared for analysis. The step of adding a liquid to the sample can be automated by integrating it into the device for automatised sample handling, resulting in saving time. Automated dosing devices can also guarantee highest standards of functional reliability.

[0013] According to a further embodiment the analytical system further comprises a transfer device for transferring the at least one closed sample container._The transfer device, which may be constituted by a suitable gripping device, can be designed to safely pick up the at least one closed sample container and transport it into the enclosure and vice versa. The transfer device is preferably designed to be adjustable so that a predetermined at least one closed sample container can be taken from, for example, a rack. The transfer device is preferably also designed to take the at least one closed sample container to the opening unit.

[0014] According to a further embodiment the transfer device is usable for shaking the at least one closed sample container. Shaking the sample inside the at least one closed sample container before analysis can have a favourable effect on the composition of certain types of samples. This is advantageous if the sample is not fully homogenised, e.g. due to the addition of an internal standard or a dilution step. In some instances, sample components may sink to the bottom of the sample container, which also results in a sample not being homogenised. If the sample is shaken beforehand, the sample is homogenised and it can be ensured that no such measurement errors occur during the analysis. If the transfer device is already capable of performing the shaking, space for a shaker can be saved and the process can be performed more quickly It would also be possible to incorporate a separate shaker alternatively. The transfer device could then place the at least one closed sample container into the shaker and pick it up again after shaking.

[0015] As noted above, the enclosure may be sealable. According to a further embodiment the enclosure is designed in a way such that it provides a tightly sealed environment for the sample. This is advantageous for contamination-free working with the sample, so that neither the sample itself can be contaminated nor the sample contaminates the work environment outside the enclosure.

[0016] According to another embodiment the enclosure is at least partially filled with argon. Argon can be used as protective atmosphere inside the enclosure. This enables the cleanest possible room to work with the sample. As argon is heavier than air it is easy to handle.

[0017] According to another embodiment the enclosure is flushable continuously or intermittently. It may be flushed with a clean gas, such as filtered air or clean argon. It is easy to perform flushing inside the enclosure as it is comparably small. Typical enclosures for sample racks need to cover more space. In the device for automatised sample handling, it may be much smaller as only the sample or samples currently to be analysed are inside the enclosure instead of a whole rack or several racks of samples.

[0018] According to a further aspect of the invention a method for automatised sample handling using an analytical system is provided. The method is carried out by several steps (some of which may be carried out) in no particular order. At least one closed sample container containing a sample is transferred from an autosampler or a sample rack to an opening unit by use of a sample handling device and / or a transfer device. The at least one closed sample container is opened by the opening unit and transferred into an enclosure. The enclosure is beneficially closed to external the sample handling device (and optionally, to the opening unit or to a remainder of the sample handling device). In implementations, the enclosure may be closed to the analytical instrument external the enclosure (the enclosure may be within the analytical instrument in some embodiments). The method optionally further comprises sealing the enclosure. In particular, the enclosure may tightly seal the at least one closed sample container within. The method may additionally comprise (at least partially) filling the enclosure with argon.

[0019] It is also possible to open the at least one closed sample container inside the enclosure, as the steps do not have to be carried out in a specific order. This gives the method flexibility and the ability to adapt to different circumstances, such as the type of analysis carried out and the nature of the sample or samples. It is possible to add an internal standard and / or a dilution fluid to the sample to standardise it and / or to improve its analysis. Opening the sample container is carried out in the immediate proximity of the analytical instrument that will be used to analyse the sample in the sample container. The distance between the analytical instrument and the sample container when it is opened may be less than 50 cm, preferably less than 25, more preferably less than 15 cm, still more preferably less than 10 cm. This distance may be measured between the sample container and a sample input opening of the analytical instrument, for example the sample input opening of the nebulizer of an analytical instrument such as a mass spectrometer.

[0020] The sample may be transferred from the sample container to the analytical instrument by a transfer line. This may be carried out by use of a sample probe that is lowered into the sample container, the sample probe being fluidly connected to the transfer line. The sample may then be transferred to e.g. a nebuliser of the analytical instrument using a very short transfer line, such as less than 50 cm, preferably less than 25 cm, in some embodiments less than 10 cm. With shortening of distances, the safety risk can be minimised. The transfer may be conducted by gas pressure transfer, for example by use of self-aspiration. In some embodiments, the transport of the sample may involve the use of a pump, such as a peristaltic pump. The sample is then converted into a fine aerosol by the nebuliser.

[0021] The sample (in the form of an aerosol) is then analysed in the analytical instrument. Controlled and consistent sample introduction is highly desirable for ICP spectral analysis. Precision delivery of samples into the nebuliser is therefore of significance. Before, during or after the analysis, the sample container may be transferred back to the sample tray or sample rack, or to another sample tray / rack that is separated from the sample tray / rack containing the samples that have not (yet) been analysed. The transfer line is then cleaned, for example by use of a washing station. The remaining sample can be disposed of or be stored up to several months depending on the sample type and on storing conditions and / or be re-used, which is of advantage for standard samples.

[0022] According to an embodiment the sample handling device is at least partially cleaned after handling of each sample. For example, the enclosure might be cleaned after handling of a sample to avoid cross contamination, but it would also be possible for other parts of the sample handling device or the device in its entirety. A clean environment for the samples is of utmost importance for minimising contamination of the samples and for occupational safety, especially when handling potentially harmful samples.

[0023] According to a further embodiment the sample is supplied to the analytical instrument by use of a liquid dosing device. Automated dosing devices can also guarantee highest standards of functional reliability. Before transferring the sample to the analytical instrument, it may be supplemented with other substances that might be helpful for the analysis.

[0024] According to a further embodiment the at least one sample container can be closed again after the analysis of the sample. For safety measures, the at least one sample container is preferably closed again. This prevents evaporation, which would make the sample unusable for reuse. In addition, no undesirable substances can get into an opened sample, which would also make it unusable for reuse. As a safety measure, the closing of the at least one sample container prevents potentially hazardous substances from entering the environment, contaminating other samples and / or affecting the health of staff.

[0025] According to a further embodiment the at least one closed sample container is surrounded by or a clean gas, such as filtered air, inside the enclosure between decapping and final capping preferably by a laminar air / gas flow. This ensures a secure transfer environment. The introduction of impurities from the ambient air into the sample can thus be avoided and, conversely, contamination of the enclosure with sample components can be prevented. As the enclosure can be smaller than conventional enclosures for sample trays, this can be carried out highly economical as a small amount of air / gas is needed.

[0026] According to a further embodiment the steps are interlaced. Interlacing can help to optimise processes and shorten the time required for handling. As a result, processes in the laboratory can be carried out more efficiently. It would be possible, for example, to carry out the opening during insertion into the enclosure. The number of steps interlacing and the duration can be customised and adapted to the circumstances best suited to the sample to be handled. The sample rack can be large and able to hold a large quantity of samples as the samples are sealed in the sample rack and only opened while handled by the device. Large quantities of samples can therefore be prepared and provided to the device for automatised sample handling by laboratory staff without having a negative effect on the sample composition or the ambient air. This can be particularly advantageous for longer measurements, such as overnight measurements.

[0027] Further features, details and advantages of the invention are apparent from the wording of the claims and from the embodiment described below with reference to the drawing.

[0028] The accompanying drawings, which are incorporated in and constitute part of this specification, illustrate embodiments of the invention and, together with the general description given above and the detailed description of the embodiments given below, serve to explain the principles of the present invention.

[0029] In the drawings:

[0030] Fig. 1 A schematic overview of a first possible arrangement of an analytical system;

[0031] Fig. 2 A schematic overview of a second possible arrangement of an analytical system;

[0032] Fig. 3 A schematic overview of a third possible arrangement of an analytical system;

[0033] Fig. 4 A schematic overview of a fourth possible arrangement of an analytical system.

[0034] Figure 1 shows a schematic overview of a possible arrangement of an analytical system. The analytical system 10 comprises a sample handling device 1 comprising an enclosure 2, an opening unit 3 and a bar code reader 4 arranged next to an analytical instrument 5. The enclosure typically has one or more openings, for example first port 21 (to the opening unit 3) and second port 22 (to the analytical instrument 5) as shown. Nonetheless and as will be discussed further below, the enclosure 2 is (or specifically, openings of the enclosure 2, for instance first port 21 and / or second port 22 are) closeable to external the sample handling device 1 (and optionally to other parts of the sample handling device 1). The enclosure 2 may be fully closeable and / or sealable in embodiments (that is, the enclosure 2 can be configured such that any paths to other parts of the analytical system, for instance provided by the one or more openings, are closed and, optionally sealed).

[0035] The opening unit 3 may be a decapper unit which is capable of removing any cap or lid of sample containers. Preferably, the opening unit 3 is also capable of closing sample containers by e.g. fitting a cap or lid onto the sample container.

[0036] A sample rack 6, which may be a sample rack of an autosampler, provides at least one closed sample container (not shown) to be analysed by the analytical instrument 5. A sample container may be, for example, a vial or any other suitable container that can be closed off. A closed sample container can be taken from the sample rack 6 by a transfer device 7. The transfer device 7 may be constituted by a gripping device configured to grip a sample container, lift it and bring it to the sample handling device 1 . The transfer device 7 may include a conveyor belt, which in turn may be provided with suitable supports for supporting sample containers. The transfer device 7 provides the sample container to the opening unit 3 via a port in the opening unit 3 (not shown). This port need not be closeable or sealable in embodiments.

[0037] The bar code reader 4 is an optional feature of the analytical system 10 but can be useful to be able to assign the samples reliably and automatically. After identifying the closed sample container via the bar code reader 4, the closed sample container is forwarded to the opening unit 3, where the closed sample container is opened. The opened sample container is then forwarded to the enclosure 2, where a sample can be taken from the sample container and be transferred to the analytical instrument. Alternatively, the sample container may be transferred from the enclosure and be placed in the analytical instrument 5 for analysis of the sample. As mentioned above, the distance between the enclosure 2 and the analytical instrument 5 can be small.

[0038] It is thus possible to carry out opening of the closed sample container inside the enclosure 2. This can help to minimise contamination or alteration risk of the sample or ambient air. It is also possible to add a standard and / or a dilution fluid for sample preparation, for example by use of an optional liquid dosing device. After the analysis carried out by the analytical instrument 5, the sample container can be closed again. This is especially advantageous if the sample should be stored and / or reused as it ensures that the composition of the sample cannot change. The sample rack 6 can provide a large quantity of sample containers which are then handled by the analytical system 10 step-by-step. This way the samples can be prepared in large batches and then be handled by use of the analytical system 10 without the risk of decrease in analysis quality or an increased risk for staff working nearby. Figure 2 shows an embodiment with the enclosure 2 of the sample handling device 1 arranged inside the analytical instrument 5 (the sample handling device 1 and analytical instrument 5 thereby being integrated in this respect). The first port 21 (between the enclosure 2 and the opening unit 3) and the second port 22 (between the enclosure 2 and the analytical instrument 5) are also shown. The opening unit 3 and the bar code reader 4 for processing the at least one sample container are arranged next to the analytical instrument in its immediate proximity to shorten the distances after opening the at least one sample container. The transfer or gripping device 7 is still able to provide the at least one sample container to the analytical system after taking it from the sample rack and vice versa.

[0039] Figure 3 shows a further embodiment of the analytical system 10 with an analytical instrument 5 and an enclosure 2 positioned next to it. The opening unit 3 and the bar code reader 4 are implemented in the enclosure 2. That is, in this embodiment the opening unit 3 and the bar code reader 4 are arranged in the interior of the enclosure 2. This reduces any contamination risk between opening unit 3 and enclosure 2. The first port 21 , which in this case is between the enclosure 2 and the transfer device 7, and the second port 22 (between the enclosure 2 and the analytical instrument 5) are also shown. In some embodiments, only the opening unit 3 can be arranged inside the enclosure 2, the bar code reader 4 being arranged outside the enclosure 2.

[0040] Figure 4 shows another embodiment of the analytical instrument 10. In this embodiment, the bar code reader 4 and the opening unit 3 are implemented in the enclosure 2 as shown in Figure 3. Additionally, the enclosure 2 is now positioned inside the analytical instrument 5 so that the sample handling device 1 is arranged inside the analytical instrument 5 in its entirety. This can help to further decrease any risk of contamination and improve work safety standards. Transfer device 7 and sample rack 6 can be arranged as in the previous embodiments. As for the embodiment of Figure 3, the first port 21 is between the enclosure 2 and the transfer device 7 and the second port 22 is between the enclosure 2 and the analytical instrument 5.

[0041] As shown, it will be understood that the enclosure 2 may have one or more openings, depending on the particular embodiment. In the embodiment of Fig. 1 , for example, the enclosure 2 has an opening provided by the first port 21 for receiving a sample container and another opening provided by the second port 22 to transfer a sample, or the sample container containing a sample, to the analytical instrument 5. The enclosure 2 is closeable. In some embodiments, at least one of these openings (and preferably, all of the openings) can be closed off by a suitable mechanism, such as a sliding and / or rotating door, so as to protect the atmosphere within the enclosure. In the embodiment of Fig. 2, the enclosure 2 may be constituted by the interior of the analytical instrument 5. The closure of the enclosure 2 (in particular, of the openings of the enclosure 2) is preferably tight and / or sealed. The enclosure 2 may be relatively small. For instance, the enclosure 2 may be sized and / or shaped to accommodate only one sample container or only a set number of sample containers (for example, in the form of a vial). In embodiments, a size of the enclosure 2 may be such that the sample container just fits. A seal of the enclosure 2 (in particular, of the openings of the enclosure 2) may be provided by rubber or plastic seals and / or strips or some other suitable sealing element.

[0042] Instead of the (optional) bar code reader 4, a non-optical device may be used, such as an RF transmitter / receiver configured for operation with transponders. In such embodiments, a sample container may be provided with a transponder instead of, or in addition to, a bar code or other optical code.

[0043] It will therefore be understood by those skilled in the art that the invention is not limited to the embodiments shown and that many modifications and additions can be made without departing from the scope of the invention as defined in the appending claims.

[0044] Reference signs

[0045] 1 Sample handling device

[0046] 2 Enclosure

[0047] 3 Opening unit 4 Bar code reader

[0048] 5 Analytical instrument

[0049] 6 Sample rack

[0050] 7 T ransfer device

[0051] 10 Analytical system 21 First port

[0052] 22 Second port

Claims

Claims1 . Analytical system (10) comprising:- an analytical instrument (5), and- a sample handling device (1), wherein the sample handling device (1 ) comprises:- an enclosure (2) for receiving at least one closed sample container, and- an opening unit (3) for opening the at least one closed sample container, wherein the enclosure (2) is configured to be closeable to outside of the sample handling device and the opening unit (3) and the enclosure (2) are located in the immediate proximity of the analytical instrument (5).

2. Analytical system (10) according to claim 1 , wherein the enclosure (2) is configured to be further closeable to the opening unit (3) or to a remainder of the sample handling device (1).

3. Analytical system (10) according to claim 1 or claim 2, wherein the enclosure (2) is configured to be further closeable to the analytical instrument (5) external the enclosure (2).

4. Analytical system (10) according to any of the preceding claims, wherein the enclosure (2) is configured to be sealed.

5. Analytical system (10) according to claim 4 wherein the enclosure (2) is designed in a way such that it provides a tightly sealed environment for the at least one closed sample container.

6. Analytical system (10) according to claim 5, wherein the enclosure (2) is at least partially filled with argon.

7. Analytical system (10) according to any of the preceding claims, further comprising a bar code reader (4).

8. Analytical system (10) according to any of the preceding claims, further comprising a liquid dosing device.

9. Analytical system (10) according to any of the preceding claims, further comprising a transfer device (7) for gripping and transferring the at least one closed sample container.

10. Analytical system (10) according to claim 9, wherein the transfer device (7) is usable for shaking the at least one closed sample container.11 . Analytical system (10) according to any of the preceding claims, wherein the enclosure (2) is continuously or intermittently flushable.

12. Analytical system (10) according to any of the preceding claims, wherein the opening unit (3) is arranged inside the enclosure (2).

13. Method for automatised sample handling using an analytical system (10), the method comprising the following steps:- transferring at least one closed sample container from an autosampler or a sample rack (6) to an opening unit (3) by using a sample handling device (1 );- opening the at least one sample container by using an opening unit (3);- transferring the at least one sample container into an enclosure (2);- closing the enclosure to external the sample handling device; and- transferring a sample from the at least one sample container to an analytical instrument (5), characterized in that the opening unit (3) and the enclosure (2) are located in the immediate proximity of the analytical instrument (5).

14. Method according to claim 10, further comprising:- analysing the sample; and / or- transferring the at least one sample container to a sample rack (6).

15. Method according to claim 10 or 11 , wherein the sample handling device (1) is at least partially cleaned after handling of the sample.

16. Method according to any of claims 10 to 12, wherein the sample is supplied to the analytical instrument (5) by using a liquid dosing device.

17. Method according to one of claims 10 to 13, wherein the at least one sample container can be closed again after analysing the sample.

18. Method according to claim 14, wherein the at least one sample container is surrounded by clean gas inside the enclosure (2) between opening and closing again.

19. Method according to claim 15, wherein the clean gas is filtered air.

20. Method according to any of claims 10 to 16, wherein the steps are interlaced.

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