Arrangement for Preparing a Plurality of Samples for an Analytical Method
20170269112 ยท 2017-09-21
Inventors
Cpc classification
B01L3/0275
PERFORMING OPERATIONS; TRANSPORTING
G01N2035/0405
PHYSICS
G01N35/10
PHYSICS
G01N35/00732
PHYSICS
B04B2011/046
PERFORMING OPERATIONS; TRANSPORTING
G01N35/1011
PHYSICS
G01N2035/1053
PHYSICS
G01N35/025
PHYSICS
B04B11/043
PERFORMING OPERATIONS; TRANSPORTING
G01N1/286
PHYSICS
B01F2101/23
PERFORMING OPERATIONS; TRANSPORTING
B01F25/10
PERFORMING OPERATIONS; TRANSPORTING
B01D35/02
PERFORMING OPERATIONS; TRANSPORTING
International classification
G01N35/02
PHYSICS
B04B11/04
PERFORMING OPERATIONS; TRANSPORTING
G01N35/10
PHYSICS
B04B5/04
PERFORMING OPERATIONS; TRANSPORTING
B01D35/02
PERFORMING OPERATIONS; TRANSPORTING
G01N35/00
PHYSICS
G01N1/28
PHYSICS
Abstract
The invention relates to an arrangement (10) for preparing a plurality of samples for an analytical method, comprising a carousel (14) with a solid housing (12) and moveable receiving parts (16) for the sample containers (18); a control for controlling the receiving parts (16) in the carousel (14); and a sample receiving device (24) for providing the sample to be analysed; one or more stations (24, 26, 28, 30, 32) for preparing samples are provided on the carousel (14), the receiving parts (16) for the sample containers (18) of the carousel (14) can be positioned on said stations; a centrifuge (22) with pairs of opposite lying receiving parts (42) provided for the sample containers (18), and said receiving parts (42) are arranged such that they can move on the centrifuge (22) and the movements can be controlled in such a manner that the sample holder (18) can be transferred between a receiving part (16) in the carousel (14) and a receiving part (42) in the centrifuge (22).
Claims
1. Assembly for taking up sample liquid from a vial and transferring the liquid to an analytic instrument, comprising: (a) a suction device; and (b) a needle or tube connected to said suction device; characterized in that (c) a filter is provided inside the needle or tube; (d) a depot with a plurality of unused needles or tubes is provided; and (e) means are provided for exchanging the needle or tube after receiving sample liquid and introducing the sample in an analytic instrument for an unused needle or tube from the depot.
2. Assembly according to claim 1, characterized by optical means for the detection of the depth of liquid supernatant above the solid state phase in the vial and means for controlling the insertion depth of the end of the needle provided at the sampling device according to the depth of the liquid supernatant.
3. Assembly according to any of the preceding claims, characterized in that the optical means for the detection of the depth of liquid supernatant above the solid state phase in the vial comprises a video camera and image processing means.
4. Assembly according to any of the preceding claims, characterized by an interface for connecting a HPLC-column, a gas chromatographic column or any other analytic instrument downline the sample taking assembly.
5. Tube or needle for use in an assembly in any of the preceding claims, characterized in that a filter is provided in its inside.
6. Tube or needle according to claim 5, characterized in that the filter is at least partly sintered by a sinter method.
7. Tube or needle according to claim 5, characterized in that the tube or needle has a wall with reduced wall thickness in the range of the filter.
8. Tube or needle according to claim 7, characterized in that the filter is provided with a filter material in the range of the wall with a reduced wall thickness and the opening there below is closed by crimping.
9. Assembly for sealing a vial present in a receptacle with a foil characterized by; (a) means for placing foil from a foil dispenser above the vial; (b) a male form movably arranged in the range above the vial; and (c) a heating for heating the male form in the range of the upper edge of the vial in such a way that the foil is welded to the edge upon pressing the male form onto the edge; (d) wherein the male form exerts a pressure on the vial when the vial is sealed.
10. Assembly according to claim 9, characterized in that the foil dispenser is provided with a reel carrying the foil.
11. Assembly according to claim 9 or 10, characterized in that the vial is adapted to be pressed on the Vortex-mixer with the male form.
12. Assembly according to claim 11, characterized in that a Vortex-mixer is provided below the vial and the vial with the receptacle is adapted to be moved in the range between the male form and the Vortex-mixer.
13. Assembly according to any of the preceding claims 9 to 12, characterized in that means are provided for expelling solvent from a vial in a receptacle by means of a gas.
14. Assembly according to claim 13, characterized in that the solvent is expelled with two hollow tubes entering the vial through the foil.
15. Sampling system for introducing samples provided on a sheet-like sample carrier into an empty or prepared vial with means for cutting the sheet-like sample carrier characterized by (a) a jet nozzle; (b) a high pressure fluid source connected to the jet nozzle; and (c) means for controlling the movement of the jet nozzle and/or the sample carrier in such a way that selected regions of the sheet-like sample carrier can be cut out.
16. Sampling system according to claim 15, characterized in that the high pressure fluid comprises at least one fluid used in the consecutive sample preparation method or measuring method.
17. Sampling system according to claim 15 or 16, characterized in that the portion of the sample carrier with the sample is cut out entirely and transferred into the vial.
18. Sampling system according to claim 15 or 16, characterized in that the portion of the sample carrier with the sample is cut out only partly and means are provided for swinging down the cut out portion in the range of the vial and means are provided for flushing the sample from the sample carrier with the fluid from the high pressure fluid source into the vial.
19. Sampling system according to claim 18, characterized in that the means for flushing the sample comprise a spraying head for spraying fluid from the high pressure fluid source onto the sample.
20. Sampling system according to any of the claims 15 to 19, characterized in that a scanner is provided for scanning the color, the degree of dryness, the position of the sample, the extent of the sample and/or further optically detectable features of the sample.
21. Sampling system according to any of the claims 15 to 20, characterized in that a housing tower is provided adapted to receive a stack of sample carriers with distance holders in-between and means for moving the sample carrier from an opening in the housing tower to the range below the jet nozzle.
22. Sampling system according to claim 21, characterized in that the opening is provided at the lower end of the housing tower and the housing tower further has an upper opening for inserting further sample carriers.
23. Sampling system according to any of the claims, characterized by a reader for reading identification data and/or data for the required sample preparation from a bar code, RFID-storage or any other data storage provided at the sample or vial.
24. Assembly (10) for the preparation of a plurality of samples for an analytical method, comprising (a) a carousel (14) with a steady housing (12) and moveable receptacles (16) for sample vials (18); (b) a control unit for controlling the receptacles (16) in the carousel (14); and (c) a sample taking device (24) for providing the sample to the analytical method; characterized in that (d) one or more stations (24, 26, 28, 30, 32) are provided at the carousel (14) for the sample preparation and receptacles (16) for vials (18) in the carousel (14) are adapted to be positioned at such stations; (e) a centrifuge (22) is provided having receptacles (42) for vials (18) which are positioned in pairs opposite to each other, and (f) the receptacles (42) for the vials (18) are moveably fixed to the centrifuge and the movements are controllable in such a way that a transfer of a vial (18) is effected between a receptacle (16) in the carousel (14) and a receptacle (42) in the centrifuge (22), (g) wherein the control is effected with the same control unit which is used to control the carousel (14).
25. Assembly according to claim 1, characterized in that the receptacles (16) for the vials (18) are arranged in a circle on the inside of the carousel (14) and the centrifuge (22) is positioned in the center of the carousel (14).
26. Assembly according to claim 24 or 25, characterized in that the receptacles (42) for vials (18) at the centrifuge (22) are formed by extendable gripping arms (40, 42) which are adjustable with respect to the rotational axis (20) of the centrifuge (22).
27. Assembly according to any of the preceding claims 24 to 26, characterized by a sampling system (24) for introducing the sample into an empty or prepared vial (18) in the carousel (14).
28. Assembly according to claim 27, characterized in that the sampling system (24) comprises an assembly for transferring samples (50) on a sheet-like sample carrier (48, 56) into a vial (18), comprising (a) a jet nozzle (58); (b) a high pressure fluid source connected to the jet nozzle; and (c) means for controlling the movement of the jet nozzle (58) and/or the sample carrier (48, 56) in such a way that selected regions of the sheet-like sample carrier (48, 56) can be cut out.
29. Assembly according to claim 28, characterized in that the high pressure fluid comprises at least one fluid used in the sample preparation method.
30. Assembly according to claim 28 or 29, characterized in that the portion of the sample carrier (48, 56) with the sample (50) is cut out entirely and transferred into the vial (18).
31. Assembly according to claim 28 or 29, characterized in that the portion of the sample carrier (48, 56) with the sample (50) is cut out only partly and means are provided for swinging down the cut out portion in the range of the vial (18) and means are provided for flushing the sample (50) from the sample carrier (48, 56) with the fluid from the high pressure fluid source into the vial.
32. Assembly according to any of the preceding claims 28 to 31, characterized in that a scanner (52) is provided for scanning the color, the degree of dryness, the position of the sample, the extent of the sample and/or further optically detectable features of the sample.
33. Assembly according to any of the preceding claims 24 to 32, characterized by one or more dispenser systems (26) for adding reagents for the sample preparation from a reservoir (62), wherein the dispensing exit (66) of the dispenser system is fixed above the vials (18) moving in the carousel (14) in such a way that the reagent can be individually introduced into selected vials.
34. Assembly according to any of the preceding claims 24 to 33, characterized in that a device (28) for sealing a vial (18) present in a receptacle (16) in the carousel (14) with a foil (68) from a foil dispenser (70).
35. Assembly according to claim 34, characterized by (a) means for placing the foil (68) from the foil dispenser (70) above the vial (18); (b) a male form movably arranged in the range above the vial; and (c) a heating for heating the male form in the range of the upper edge of the vial in such a way that the foil is welded to the edge upon pressing the male form onto the edge; (d) wherein the male form exerts a pressure on the vial when the vial is sealed.
36. Assembly according to any of the preceding claims 24 to 35, characterized in that a Vortex-mixer (30) is provided below the vials movable in the carousel and means for pressing the vial on the Vortex-mixer.
37. Assembly according to claims 35 and 36, characterized in that the vial is adapted to be pressed on the Vortex-mixer (30) with the male form.
38. Assembly according to any of the preceding claims 24 to 37, characterized in that a heating (73) for heating one or more vials is provided in the carousel.
39. Assembly according to any of the preceding claims 24 to 37, characterized in that means (67) are provided for expelling solvent from a vial in a receptacle in the carousel (14) by means of a gas.
40. Assembly according to any of the preceding claims 24 to 38, characterized in that the sample taking device for providing the sample for the analytic method comprises: (a) a suction device (114); and (b) a needle (84) connected to said suction device; (c) a filter inside the needle (84); (d) a depot (90) with a plurality of unused needles; and (e) means for exchanging the needle after receiving sample liquid and introducing the sample in an analytic instrument for an unused needle from the depot.
41. Assembly according to any of the preceding claims 24 to 40, characterized by optical means for the detection of the depth of liquid supernatant above the solid state phase in the vial and means for controlling the insertion depth of the end of the needle provided at the sampling device according to the depth of the liquid supernatant.
42. Assembly according to any of the preceding claims 24 to 41, characterized by a reader (36) at the carousel for reading identification data and/or data for the required sample preparation from a bar code, RFID-storage or any other data storage provided at the sample or vial.
43. Assembly according to any of the preceding claims 24 to 42, characterized in that an interface (94) for connecting a HPLC-column, a gas chromatographic column or any other analytical instrument is provided downline the sampling device.
44. Assembly according to claim 43, characterized in that an opening (92) is provided in the range of the receptacles for vials provided at the centrifuge (22) in the bottom of the carousel which connects the carousel to a waste container.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DESCRIPTION OF AN EMBODIMENT
[0084]
[0085] A centrifuge 22 is arranged in the center portion of the carousel. The centrifuge 22 also rotates about the center axis 20. Various stations for sample preparation are provided outside along the housing, including a station for sample introduction and sample taking. A sampling system 24 for introducing dried samples from a sheet-like carrier is one of said stations. The next station in a clockwise direction has three dispensing systems 26 for dispensing reagents for sample preparation from a reservoir. The next station 28 in a clockwise direction is a foil dispenser for sealing a vial 18 present in a receptacle 16 in the carousel 14 with a foil. A Vortex-station 30 is positioned below the foil dispenser 28. The Vortex-station 30 can be well seen in
[0086] A sample taking device 32 is positioned on the side opposite to the sampling system 24. The taken samples which are readily prepared are transferred to an analytic instrument, which is a HPLC-column with a detector (not shown) in the present embodiment.
[0087] All stations and devices described above are connected to a common control unit (not shown). The control unit controls all required drivers and actuators and receives and stores data and results. Settings can be either directly made at the station or with a user-interface at the control unit. Sample preparation methods with kind and duration of the individual sample preparation steps can be inserted and stored.
[0088]
[0089] The vials 18 are held in the receptacles 16. Each vial 18 has the form of a test-tube and is provided with a bar code 38, which is stuck to the vial 18 in the form of a printed sticker. On the outside, the housing 12 has an ordinary barcode scanner 36. The scanner 36 serves as a reader and reads the data stored in the barcode. In the present embodiment such data comprise an identification number. The identification number relates to the kind of sample, such as blood or urine, and a specific sample preparation method. The scanner 36 transfers the position, i.e., the angular position of the receptacle 16 in the carousel 14 and the identification number to the control unit. The control unit determines the required sample preparation steps using such identification number and moves the vial to the individual stations.
[0090] The samples in the vials 18 can move along the stations in the order of their positions. However, there are cases where some stations need not be used, where a station is occupied or where a sample shall be treated with higher priority. For this purpose the vial can be shifted with gripping arms 40 of the centrifuge 22 to another receptacle 16. For this purpose the gripping arms 40 are adapted to be moved in a radial direction. They are extended from a holder 41 which rotates together with the actuator. They can be extended as far as the carousel. A pliers-shaped gripper 42 is provided at the end of the gripping arms 40 which is adapted to grip the vial 18 and hold it. Suitable actuators with sliding contacts for power supply are provided for each gripping arm 40 and each gripper 42. By slowly rotating the centrifuge 22 a vial 18 can be moved from one receptacle to another receptacle 16.
[0091] In the present embodiment two gripping arms 40 are shown at the centrifuge 22. However, it is also possible to provide several pairs of opposite gripping arms 40. In any case the centrifuge 22 has a double function: first, samples can be exposed to centrifugation as with common centrifuges. This is shown in
[0092]
[0093] Each sample carrier 48 is provided with a bar code 54. The bar code 54 is read by a common bar code scanner 52 or a camera. The data are transmitted to the control unit for tracking. If there are several samples, several bar codes may be provided. The same scanner 52 is used to determine the exact position of the samples 50 on the sample carrier. The scanner 52 operates with different wavelengths of the optical spectrum and can thereby also detect the kind of sample. Samples with an undesired or unknown appearance can be excluded from the sampling in order to avoid contamination of the assembly. It is also possible to determine the position with a further scanner or to use a pre-set position.
[0094] The lowest sample carrier 56 is moved in the range above a vial 18. A suitable actuator (not shown) is provided for this purpose. The actuator is an x-y-actuator and the holder for the sample carriers is mounted thereon. The actuator enables, therefore, not only a horizontal movement of the sample carrier 56 in a direction perpendicular to the housing 46 but also in a lateral horizontal direction which is parallel to the front end of the housing wall.
[0095] A high pressure jet nozzle 58 is held at the front housing wall of the housing 46. This is shown in
[0096] The solvent is a solvent which is used anyway in the further proceedings of sample preparation. Therefore, it need not necessarily removed from the vial which would involve a certain effort.
[0097] Depending on the application and the kind of sample carrier, several samples may be cut out simultaneously. In the present embodiment two adjacent samples 50 are cut out with two adjacent high pressure jet beams. For this purpose two high pressure jet nozzles 58 are provided in the housing 46.
[0098] In an alternative embodiment which is not shown here, the high pressure jet nozzle is moved instead of the sample carrier 56. However, the same result is obtained at all times.
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[0100] In the present embodiment three dispensing systems 26 are provided which can operate simultaneously. In such a way the same reagent can be dispensed into three vials at the same time. Thereby, a high dispensing rate is achieved. Depending on the application, however, it is also possible to use different reagents for different applications or sample preparation methods.
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[0103] For sealing the vial 18 a section of unused foil is unrolled. A reel 82 with an actuator (not shown) is provided at the lower end of the foil for this purpose. The unused foil is placed between the male form 78 and the edge 80. The holder 72 is then moved downwards with the arm 74 and the heated male form 78 connected thereto. For this purpose an actuator (not shown) is provided. The actuator is controlled by the control unit. Due to the pressure and the increased temperature, the foil is welded to the edge. The foil in the range of the vial is released from the remaining foil 68. The vial 18 is tightly sealed. The welding is carried out in a way which avoids the entering of fumes into the vial.
[0104] Depending on the application the vial 18 can be further pressed down. Vortex-station 30 is positioned below the vial 18 and the male form 78. Upon exerting a pressure on the vial 18 the Vortex-movement is carried out. The sample in the vial 18 is mixed (vortexed).
[0105] Depending on the desired sampling rate, a plurality of foil dispensers 28 can be arranged in a series. In this case several vials 18 can be sealed simultaneously. Alternatively, only a plurality of male forms is used which seal several vials 18 simultaneously using a wider foil. In the present embodiment two foil dispensers 28 are used with two foils (see
[0106] A heating 73 is provided next to the Vortex-Station 30. This is shown in
[0107] For separating solid particles, two of the vials 18 are gripped with opposite gripping arms 40 of the centrifuge 22 and rotated.
[0108] A sample taking device 32 is provided for taking a sample and transferring it to the analytic instrument. This is shown in
[0109] Filter material 88 is present in the hollow needle 84. This can be seen in
[0110] If sample liquid is sucked into the hollow needle 84 solid particles and floating particles are held back in the filter material 88. A piston pump 114 is provided for this purpose. The sample prepared in such a way can be directly introduced in a HPLC column or any other analytical instrument.
[0111] A fresh needle with unused filter material is used for each sample. They are stored in a depot 90 with an ejector. Therefore, the used needle is released before a new sample can be taken and a fresh needle is fixed to the head.
[0112] The sample from the vial 10 is transferred to the analytical instrument with the sample taking device 32. In the present embodiment a chromatographic column (not shown) is used for the analysis. A rotary valve 94 having 6 ports 96, 98, 100, 102, 104 and 106 is used for this purpose. A measuring device, a pump and a filter needle is connected to the rotary valve. This is shown in
[0113] Eluent from an eluent source is added at port 98. This is represented by an arrow 108. Port 100 is connected to a chromatographic column. In the present embodiment a HPLC column, not shown, is used. This is represented by an arrow 110. Port 102 is connected to the port 112 of a piston system 114 through pipe 116. The piston system 114 is operated with a stepper motor 118. This is represented by an arrow 120. Port 96 is connected to a second port 124 of the piston system 114 through pipe 122.
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[0115] A well-defined volume of sample liquid 128 is sucked through the needle 84 to the port 104 and through the port 102 to the pipe 116 which has the form of a loop. Dead volume of the needle and the valve are well considered therein.
[0116] The valve is then moved to the position shown in
[0117] For flushing, the valve is rotated back as shown in
[0118] After sample taking and flushing of the valve, the needle 84 is released and dropped into the vial and the vial 18 is gripped with the gripping arm 40 of the centrifuge 22 and transferred to an opening 92 in the bottom of the housing 12 by opening the grippers 42 above the opening 92. This is illustrated in
[0119] By moving the piston to the right in the representation the next sample can be sucked up and the cycle can be repeated.
[0120] The control unit is provided in a housing together with a power supply and the required electronic components, for example next to or under the housing 12. The housing is well aired and shielded against chemicals and vapors. With the control unit samples of higher priority can be treated more quickly during sample preparation even if the system is already occupied with different samples. A sensor can identify idle positions, count them and report them to the control unit. When inserting the vials the user can enter the amount of needed positions with the accompanying priority. They are then adequately considered by the control unit. Samples with contents which cannot be analyzed by the system in the present configuration will be returned without any treatment. In such a way excessive contamination is avoided.
[0121] Temperatures in the male form 78 and in the heating, the rotational speed and the angle at the centrifuge, the dispensing volumes and the kind and order of the sample preparation can be adjusted with the control unit. The control unit also processes and displays signals of sensors, cameras and scanners.