• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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  • 优先权
    • 专利摘要:
    SAMPLING DEVICE AND METHOD. An automatic in situ sampling method and associated sampling device for capturing a sample of material from a container. The methods of the present invention make use of a sampling device having an extensible sample capture element (60) with a concave sample capture pocket (65) located near a distal end (60b). The sample capture pocket is adapted to capture a known volume of material when the sample capture element is extended into said material. The sample of material remains trapped in the sample capture pocket after the sample capture element retracts. The ports (75) in the sample capture pocket can be placed in communication with the corresponding material transfer channels extending through the sample capture element to allow in situ processing of a sample of material, and the subsequent discharge of the sample. sample to an analyzer or other downstream location.
    公开号:BR112012032727B1
    申请号:R112012032727-5
    申请日:2011-06-21
    公开日:2020-06-30
    发明作者:Peter Alfred Blacklin；Wayne Fowler, JR.；Joel Michael Hawkins；Ii Howard William Ward
    申请人:Mettler-Toledo Gmbh；
    IPC主号:
    专利说明:

    [0001] [001] The present invention relates to a device and method for acquiring a sample of material. More particularly, the present invention relates to a method of acquiring a sample of material, such as a reaction / reagent sample, using a sampling device having an extensible sample capture element.
    [0002] [002] As would be obvious to those skilled in the art, there are several situations and / or processes for which it would be desirable to extract a sample of a material from a container in which the material is contained. Such extraction would generally be desirable for the purposes of examination and testing, but it can be performed for other reasons, too.
    [0003] [003] With respect to process monitoring, such sample extraction may be desirable in several processes, including, without limitation, applications of parallel synthesis (combinatorial chemistry), organic synthesis, chemical process development, and scale-up of laboratory in production. Several other similar applications where sample extraction would be of interest also exist and would be known to those skilled in the art.
    [0004] [004] The known sampling devices can be operated manually, or they can employ a vacuum-based device mounted remotely or in a container containing a material of interest, or a bypass port or similar mechanism through which the amount of a material of interest can be expressed. In any case, however, known methods generally require that an extracted sample be removed from the container and then transferred to another container before the sample can be cooled or operated.
    [0005] [005] Known manual sample capture and analysis methods commonly suffer from a lack of precision with respect to sample capture timing and subsequent sample processing. In addition, sample capture methods can be used only to create samples that are at atmospheric pressure. Reactions that occur under pressure cannot be sampled by these techniques. A sample capture method that makes use of a type of sampling device override, where the reaction flows through a circuit to a point where it can be sampled, can be used to sample reactions under pressure - however, a large volume reaction is necessary to use such a device.
    [0006] [006] Importantly, known sample capture methods also do not allow sample processing (mixing, cooling, dilution, etc.) to take place substantially simultaneously with sample capture, but instead require a sample first be transferred to another container. Consequently, the state of a given sample may actually change from the moment of sample extraction to the moment of cooling, etc.
    [0007] [007] Therefore, based on these problems above with known sampling methods, it should be apparent that a method of capturing a material sample and for processing the material sample in situ and substantially simultaneously with the sample capture would be desirable . A sample capture device and method of the present invention allows for such a process.
    [0008] [008] The modalities for sampling devices that can be used in accordance with the present invention can be arranged as elongated probes having extensible sample capture elements. Among other things, a sampling device of the present invention can be used to sample small reaction volumes (for example, from 5 to 100 μl), and to extract a sample from within a reaction volume. Since a sampling device of the present invention is a sealed unit, it can also be located through a door within a pressurized reaction chamber or evacuated to sample a pressurized reaction volume. A sampling device of the present invention can also be used over a wide temperature range (for example, - 40 C to 150 C).
    [0009] [009] Unlike known sample capture methods, the methods of the present invention allow for substantially simultaneous sample capture and sample processing (e.g., cooling, dilution, mixing, etc.). Therefore, the practice of the present invention minimizes or eliminates any change in sample conditions between sample capture time and sample processing. This is not possible with devices or methods currently known to the inventors.
    [0010] [0010] In one embodiment, a sampling device of the present invention can include a hollow and substantially cylindrical outer tube of some length. A proximal end of the outer tube can be attached or otherwise attached to a body part of a probe driver assembly. Concentricly arranged inside the outer tube at a distal end is a set including an outer sleeve, an inner sleeve and an extendable sample capture element. A substantially frustoconical adapter is attached to the distal end of the outer tube and tapers to a reduced diameter that approximates the diameter of the outer sleeve.
    [0011] [0011] Both the outer sleeve and the inner sleeve are held in position by the adapter, which presses an upper shoulder of the inner sleeve collar tightly against the distal face of the outer tube when attached to it. Consequently, when the adapter is fully mounted on the outer tube, the inner sleeve and the outer sleeve are held together and are also prevented from carrying out movement with respect to the outer tube and the adapter.
    [0012] [0012] The sample capture element is located to be reciprocating to the inner sleeve. The outer diameter of the sample capture element is provided to be close in dimension to the inner diameter of the inner sleeve, so that a tight but sliding fit is produced between them. When the sample capture element is in a retracted (closed) position, the distal end can be positioned substantially even with the distal ends of the inner sleeve and outer sleeve. When the sample capture element is in an extended (sampling) position, the distal end can protrude from the distal end of the outer sleeve. The sample capture element is provided with a concave sample capture pocket that, during extension of the sample capture element, is exposed to and captures a quantity of a sample of interest.
    [0013] [0013] A proximal part of the sample capture element extends into the increased inner diameter of the proximal part of the inner sleeve. The proximal end of the sample capture element is received within the distal end of the substantially hollow inner tube which is concentricly disposed within the outer tube. The outer diameter of the inner tube approaches the inner diameter of the proximal part of the inner door sleeve so that a tight but sliding fit is produced between them. The sample capture element is retained in the inner tube, such as by a pin.
    [0014] [0014] In an illustrative automated mode (automatic sampling) of a device of the present invention, a proximal end of the inner tube extends through the proximal end of the outer tube and is connected to a driver (for example, pneumatic cylinder) that provides the desired extension and retraction of the sample capture element. In an illustrative (manual) manually operated modality of a device of the present invention, the inner tube can be connected in a similar way to a manually operated lever mechanism or linearly driven plunger that provides the desired extension and retraction of the capture element. sample when manually triggered by a device user.
    [0015] [0015] During the extension and retraction of the sample capture element, the sample capture element is oriented by the contact between its exterior and the interior of the distal part of the inner door sleeve, in addition to by contact between the exterior of the inner tube and the interior of the proximal part of the inner door sleeve. The proper linear movement of the sample capture element is thus guaranteed. Rotation of the sample capture element during reciprocation can be prevented if desired.
    [0016] [0016] The sample capture element is opened to allow purging / ventilation and to allow in situ processing (mixing, dilution, cooling, etc.) of material samples while located in the sample capture pocket. In particular, the sample capture pocket is provided with a supply port and a vent / vent port, each of which is associated with a corresponding channel that runs through the sample capture element and exits through the proximal end. Sample lines (for example, piping) can be connected to each of these supply and / or purge / ventilation channels to take processing materials to the sample capture pocket and to allow ventilation and allow material to be purged from the sample capture pocket. Such piping can be routed through the inner tube. The distal part of the inner sleeve is provided with partitions that allow the ports in the sample capture pocket to communicate with the corresponding channels in the sample capture element during a processing cycle (for example, mixing, dilution, cooling) or purge / ventilation.
    [0017] [0017] The channels in said sample capture element are internal to the same or the channels in said sample capture element extend along its external surface.
    [0018] [0018] In another illustrative embodiment, the design described above can be changed to have a smaller number of individual components. Particularly, in this alternative modality, the internal and external sleeves and the adapter of the modality described previously are combined in a single element. This element forms an end cap that leads into the distal end of an external tube and acts as a reciprocating guide and protective cover for the sample capture element. The end cap contains internal channels or grooves that connect the sample capture element pocket ports to the sample capture element channels.
    [0019] [0019] During the use of these modalities, the distal end of the device is typically immersed in or kept close to the surface of a material from which a sample is to be extracted. At the desired time, the sample capture element is extended into the material, where a quantity of material fills the sample capture pocket and remains there as the sample capture element is subsequently retracted back into position closed. With the sample of the material trapped in the sample capture pocket, the sample can be processed, such as by contacting the sample with a cooling or diluting substance in order to stop a reaction in progress and dilute the sample, before transferring the sample of material to another device or container.
    [0020] [0020] When a sample capture element of a sampling device of the present invention is extended into a reaction volume to capture a sample, the sample lines are typically empty, having been purged, for example, with a gas or with a liquid that is neutral to the reaction being sampled. As will be apparent, when the sample capture element extends into the reaction volume, any material inside the sample capture pocket will come in contact with the reaction materials.
    [0021] [0021] The choice of purge material may vary depending on the reaction being sampled. For example, a gas purge material may not be ideal if the reaction volume is small and the reaction is under pressure, since the purge gas can cause a fluctuation in the reaction pressure. Similarly, any fluid present in the sample capture pocket when the sample capture element extends will mix quickly with the reaction materials. It must also be considered that the remnants of any cooling medium may compromise a reaction.
    [0022] [0022] While the sample capture element is extended, the sample lines that were previously empty, can be filled with cooling medium. The flow path through the sampling device may include transfer ports and an overflow groove in the sample capture element to allow flow in the fluid circuit when the sample capture element is in an extended position.
    [0023] [0023] In the case of the illustrative modalities mentioned above, the door partitions of the inner sleeve (or combined element) align with the transfer ports of the sample capture element as the sample capture element reaches full extension, allowing flow through the overflow groove and channels and within the sample line circuit. The cooling medium can therefore be introduced into the sample capture element and possibly put under pressure while the sample capture element is still extended. In this way, the cooling medium is available to immediately flow into the sample capture pocket and mix with the captured material sample by retracting the sample capture element and aligning the sample capture pocket doors with the partitions. of the inner sleeve.
    [0024] Therefore, unlike the known devices and methods, sample processing according to the present invention can take place while the captured sample is still in the sampling device (i.e., in situ). In addition, by providing a supply of cooling medium or other material, sample processing can be started immediately by retracting the sample capture element. This ensures that the captured sample is preserved in a condition that is as close as possible to the sample volume condition from which it will be extracted.
    [0025] [0025] In addition to the features mentioned above, other aspects of the present invention will be readily apparent from the following descriptions of the drawings and illustrative modalities, where similar numerical references across the various views refer to identical or equivalent features, and where:
    [0026] [0026] Figure 1 is an exploded view of part of an illustrative embodiment of an automatic sampling device of the present invention;
    [0027] [0027] figure 2a is an enlarged view in partial transparency of a distal part of the automatic sampling device of figure 1 with a sample capture element in a retracted (closed) position;
    [0028] [0028] figure 2b illustrates the distal part of the automatic sampling device of figure 2a with the sample capture element in an extended position (sampling);
    [0029] [0029] figure 3 is an enlarged view of a distal end of an illustrative sample capture element of the present invention, where a sample capture pocket with door is visible;
    [0030] [0030] figure 4a is an enlarged cross-sectional view of the distal part of the automatic sampling device of figure 1, in which the sample capture element is in a retracted (closed) position and a first liquid flow path (mode of collection) is illustrated;
    [0031] [0031] figure 4b illustrates a distal part of the automatic sampling device of figure 4a with the sample capture element in an extended position (sampling) and a second liquid flow path (overflow mode) is illustrated;
    [0032] [0032] figure 5 shows the sample capture device of figures 1 to 4b in a fully assembled condition;
    [0033] [0033] figure 6a illustrates an assembled distal part of an alternative illustrative embodiment of an automatic sampling device of the present invention, with an associated sample capture element in a retracted (closed) position;
    [0034] [0034] figure 6b illustrates the automatic sampling device of figure 6a with the sample capture element in an extended position (sampling);
    [0035] [0035] figure 7 is a cross-sectional view of a distal part of the automatic sampling device illustrated in figures 6a and 6b;
    [0036] [0036] figure 8 is an enlarged perspective view of an illustrative sample capture element that can be used with the automatic sampling device of figures 6a and 6b and figure 7;
    [0037] [0037] figure 9a is a transparent view showing an alternative embodiment of a sample capture element and an associated sleeve of the present invention, with the sample capture element in an extended position;
    [0038] [0038] figure 9b is an enlarged view of part of the sample capture and sleeve element of figure 9a;
    [0039] [0039] figure 10a is a transparent view illustrating the sample capture element and associated sleeve of figure 9a in a retracted position;
    [0040] [0040] figure 10b is an enlarged view of part of the sample capture and sleeve element of figure 10a;
    [0041] [0041] figure 11 is an isometric view of an illustrative embodiment of a manually operated (manual) sampling device of the present invention;
    [0042] [0042] figure 12 is a front view of the manual sampling device of figure 11 with connections to a material introduction device and a sample collection container shown schematically;
    [0043] [0043] figure 13 is a process diagram illustrating an illustrative method of operating an automatic sampling probe of the present invention; and
    [0044] [0044] figure 14 is a process diagram illustrating an illustrative method of operating a manual sampling probe of the present invention.
    [0045] [0045] An illustrative embodiment of a sampling device 5 of the present invention is illustrated in figures 1 to 5. In that case, the device is an automatic sampling device 5, as explained in greater detail below. However, such a design can also be used substantially in a manually operated (manual) version of a sampling device according to the present invention. A partial inventory of the components of that device 5 is illustrated in the exploded view of figure 1.
    [0046] [0046] As illustrated, this automatic sampling device 5 includes a hollow and substantially cylindrical outer tube 10 of any desired length. A proximal end 10a of the outer tube 10 can be attached or otherwise affixed to a body part 255 of a probe driver assembly 250, as shown in figure 5. A distal end 10b of the outer tube 10 is screwed in as shown. In this case, the threads 15 are arranged externally in the outer tube 10, although the internal thread can be supplied in other modalities. The outer tube 10 can be constructed from various materials depending on the substances to which it can be exposed. It has been found, however, that a HASTELLOY alloy, such as HASTELLOY C-22 or C-276, is particularly well suited for this purpose. HASTELLOY alloys are available from Haynes International, Inc.
    [0047] [0047] Arranged concentric within a distal part of the outer tube 10 is a sample capture assembly 20 that includes an outer sleeve 30, an inner sleeve 40, an extendable sample capture element 60 and an adapter fixation 25.
    [0048] [0048] The fixing adapter 25 of that particular automatic sampling device 5 is substantially frustoconical in shape, with a proximal part 25a in diameter larger than a distal part 25b. The proximal end of the adapter 25 is internally screwed to engage the distal threaded end 10b of the outer tube 10. The external thread can be provided in other embodiments having an internally threaded outer tube. Preferably, but not essentially, the adapter 25 of that automatic sampling device 5 is constructed from the same material as the outer tube 10.
    [0049] [0049] The outer sleeve 30 is constructed as an elongated hollow tube of some length, with a collar 35 of increased diameter surrounding its outer proximal end 30a. The outer sleeve 30 is received in the adapter 25 and positioned there by contact of a lower shoulder formed by the collar 35 of the outer sleeve 30 and a corresponding shoulder 27 formed in the adapter (see figures 4a and 4b). In this embodiment of the automatic sampling device 5, a distal part 30b of the outer sleeve 30 extends through the small diameter opening in the adapter and projects from there for a predetermined distance. Preferably, the inner diameter of the distal part 25b of the adapter 25 and the outer diameter of the outer sleeve part 30 that passes through it have dimensions that produce a sliding fit between them.
    [0050] [0050] The outer sleeve 30 can be constructed from various materials depending on the materials to which it is exposed. In this particular embodiment, the outer sleeve 30 is constructed of stainless steel.
    [0051] [0051] The inner sleeve 40 is also constructed as an elongated hollow tube of some length. The inner sleeve 40 includes a proximal part 40a having an inner and outer diameter that is greater than the inner and outer diameter of a distal part 40b. The distal and proximal parts 40a, 40b of the inner sleeve 40 are separated by a collar 45 that forms a lower outer shoulder 50 and upper inner and outer shoulders 55, 57. The distal portion 40b of the inner sleeve 40 is received and resides within the inside of the outer sleeve 30. The outer diameter of the distal part 40b of the inner sleeve 40 and the inner diameter of the outer sleeve 30 are each of a dimension that resets in a sealing fit therebetween.
    [0052] [0052] As illustrated in figures 4a and 4b, the longitudinal position of the inner sleeve 40 within the outer sleeve 30 is configured by the contact between the lower shoulder 50 of the inner sleeve collar 45 and the proximal end 30a and the collar 35 of the outer sleeve 30. Preferably, the length of the distal part 40b of the inner sleeve 40 is such that the distal ends of the inner sleeve and outer sleeve 30 are aligned when the inner sleeve is installed in the outer sleeve.
    [0053] [0053] The inner sleeve 40 can be constructed from various materials depending on the substances to which it will be exposed. In this particular embodiment, the inner sleeve 10 is constructed of a polytetrafluoroethylene (PTFE) material, such as a TEFLON material available from DuPont. An advantage of using a material such as TEFLON is that it is inert to most chemicals and has a low coefficient of friction.
    [0054] [0054] It was also found that the natural elasticity of PTFE allows it to create a good seal between the outer sleeve 30 and a sample capture element 60 of the automatic sampling device 5. More particularly, the elastic-plastic behavior of such material allows fair normal manufacturing tolerances to be applied. In this case, the orifice of the inner sleeve 40 can be made smaller than the outer diameter of a sample capture element 60 described in greater detail below, which reciprocates in it, however when two components are fitted together the TEFLON deforms in the internal orifice and burnishes (ie, local poly deformation to the inner surface of the inner sleeve) during installation. Preferably, the inner diameter of the sleeve 40 is selected to keep the outer fibers in an elastic state (until higher temperatures are reached) so that the sleeve provides a compressive sealing force against the sample capture element, thereby sealing the transfer passages and passages against communication with the adjacent passages.
    [0055] [0055] When the adapter 25 and the inner and outer sleeves 30, 40 are installed on the distal end 10b of the outer tube 10, the larger diameter proximal part 40a of the inner sleeve 40 extends into the distal end of the outer tube 10. The outer diameter of the proximal part 40a of the inner sleeve 40 and the inner diameter of the outer tube 10 are each of a dimension that preferably results in a sealing fit between them.
    [0056] [0056] Both the outer sleeve 30 and the inner sleeve 40 are held in place by adapter 25, which presses the upper outer shoulder 57 of the inner sleeve collar 45 against the distal face of the outer tube 10 when the adapter is screwed on in the outer tube. The adapter 25 acts as a fixing device to retain the outer sleeve 30 and the inner sleeve 40 and to seal the outer tube 10 with the collar 45 of the inner sleeve collar 40. At the same time, the inner sleeve 40 and the outer sleeve 30 also they are held tightly together and are prevented from making the longitudinal (linear) movement with respect to the external tube 10 and the adapter 25.
    [0057] [0057] As mentioned above, the sample capture set 20 also includes a sample capture element 60. The sample capture element 60 is located to reciprocate within the inner sleeve 40, as can be better understood by reference to figures 2a and 2b and 4a and 4b. For this purpose, the outer diameter of the sample capture element 60 and the inner diameter of the distal part 40b of the inner sleeve 40 have a dimension that produces a sealing fit, but slidably oriented between them.
    [0058] [0058] The length of the sample capture element 60 may vary depending on the length of the outer tube 10 and / or other components of the automatic sampling device 5. Preferably, the length of the sample capture element 60 is at least sufficiently so that the proximal end resides within the proximal part 40a of the inner sleeve 40, if the sample capture element 60 is in an extended or retracted position.
    [0059] [0059] When the sample capture element 60 is in a retracted (closed) position, as shown in figures 2a and 4a, the distal end 60b is preferably positioned substantially homogeneously with the distal ends of the inner sleeve 40 and the sleeve outer 30. When the sample capture element 50 is in an extended (sampling) position, as shown in figures 2b and 4b, the distal end 60b projects from the distal ends of the inner sleeve 40 and outer sleeve 30 for some distance predetermined.
    [0060] [0060] As more clearly illustrated in figure 3, the sample capture element 60 is provided with a concave sample capture pocket 65 which, during the extension of the sample capture element, is exposed to and captures a quantity of a sample in which the distal end of the automatic sampling device 5 is immersed. Sample capture pocket 65 can be supplied in different sizes to capture different sample volumes (aliquots).
    [0061] [0061] The sample capture element 60 can be constructed from various materials depending on the substances to which it will be exposed. In this particular embodiment, the sample capture element 60 is constructed of a ceramic material. The sample capture elements of the embodiments of the present invention can be resistant to strong acids and strong caustics.
    [0062] [0062] Sample capture element 60 is opened to allow purging / ventilation and to allow cooling of material samples located in sample capture pocket 65. In particular, sample capture pocket 65 is provided with a cooling port 70 and a bleed / vent port 75, each of which is associated with a corresponding channel 80, 85 which runs through the sample capture element 60 and exits through the proximal end 60a. The distal part 40b of the inner sleeve 40 is provided with partitions 90 that allow ports 70, 75 in the sample capture pocket 65 to communicate with the corresponding channels 80, 85 in the sample capture element 60 during a cooling cycle and / or purge / ventilation.
    [0063] [0063] The sample capture element 60 can also be provided with an override groove 240 which is located in fluid communication with transfer ports 80b, 85b of channels 80 and 85 on the sample capture element by partitions 90 in inner sleeve 40 to allow circulation of a cooling medium while the sample capture element is in an extended position. This allows the sample lines and channels 80, 85 in the sample capture element 60 to be filled with recirculating cooling medium as illustrated in figure 4b. The cooling medium can therefore be introduced into the sample capture element 60 and possibly put under pressure while the sample capture element is in an extended position. In this way, the cooling medium is available to immediately flow into the sample capture pocket 65 and mix with a captured sample by retracting the sample capture element and aligning the sample capture pocket doors 70, 75 with partitions 90 of the inner sleeve.
    [0064] [0064] As illustrated in figure 5, tubing 95 or similar duct can be connected to each of the cooling and purge / ventilation channels 80, 85 to take the cooling materials to the sample capture pocket 65, and to allow vent and allow material to be purged from the sample capture pocket. When flexible plastic tubing is used for this purpose, the ends of the tubing 95 can be preformed with threads by techniques known to those skilled in the art, the threaded ends can be subsequently trimmed to provide a uniform face for the threaded tube end, and the screwed ends of the tubing can be engaged with similar threaded sections provided at the proximal ends of channels 80, 85. By screwing the tubing into associated channels in the sample capture element, the screwed ends of the tubing flush with the pilot diameter of the channels thus producing a seal. Such tubing 95 can be directed through an inner tube 100 (described in more detail below) of the automatic sampling device 5.
    [0065] [0065] The proximal end 60a of the sample capture element 60 extending into the proximal part 40a of the inner sleeve 40 is received within the distal end 100b of a substantially hollow inner tube 100 which is concentrically disposed within the outer tube 10. As best illustrated in figures 4a and 4b, the outer diameter of the inner tube 100 approximates the inner diameter of the proximal part 40a of the inner sleeve 40, so that a sealed but sliding fit is produced between them.
    [0066] [0066] In this embodiment, the proximal end 60a of the sample capture element 60 is retained at the distal end 100b of the inner tube 100 by a pin 105 that passes through corresponding holes in both components. As illustrated in figure 5, the proximal end 100a of the inner tube 100 extends through the proximal end 10a of the outer tube 10 and is connected to an actuator 260 that provides the desired extension and retraction of the sample capture element 60.
    [0067] [0067] With reference to figure 4a, it can be seen that when the sample capture element 60 is in a retracted position, a space 110 exists between the distal end 100b of the inner tube 100 and the upper inner shoulder 55 of the inner sleeve 40 The length of this space 110 represents the maximum possible length of the extension of the sample capture element 60 since, as illustrated in figure 4b, the contact between the distal end 100b of the inner tube 100 and the upper inner shoulder 55 of the inner sleeve 40 will act as a hard stop with respect to the sample capture element extension 60. Of course, the driver 260 may also have a pitch that is less than the length of the gap 110, in which case the contact between the distal end 100b of the inner tube 100 and the upper inner shoulder 55 of the inner sleeve 40 may not occur.
    [0068] [0068] During the extension and retraction of the sample capture element 60, the sample capture element is oriented by contact between its outer surface and the inner surface of the distal part 40a of the inner sleeve 40, in addition to by contact between the surface outer of the inner tube 10 and the inner surface of the proximal part 40a of the inner sleeve 40. The proper axial linear movement of the sample capture element 60 is thus guaranteed.
    [0069] [0069] It may be desirable to prevent rotation of the sample capture element 60 so that the repeated orientation of the sample capture pocket 65 during the extension of the sample capture element can be guaranteed. As illustrated in figures 4a and 4b, rotation of the sample capture element 60 of this embodiment of the automatic sampling device 5 is prevented by causing the ends of the sample capture element / inner tube 105 to extend inward. of linearly arranged partitions 115 in the proximal part 40a of the inner sleeve 40 (see figure 1). Consequently, the sample capture element 60 can reciprocate along the longitudinal geometric axis of the automatic sampling device 5, but is prevented from rotating with respect to it.
    [0070] [0070] When using the automatic sampling device 5, at least the distal end of the projected outer sleeve 30 is typically immersed in a material from which a sample is to be extracted. The depth of the material only needs to be sufficient to cover the extended part of the sample capture element. At the desired time, the driver 260 is activated to extend the sample capture element 60 as described above. This causes the sample capture element 60 to enter the material to be sampled, where a quantity of material fills the sample capture pocket 65 and remains there as the trigger 260 is subsequently activated to retract the sample capture element. sample back to its closed position.
    [0071] [0071] With the material sample trapped in the sample capture pocket, the sample can be cooled with a cooling medium, as shown in figure 4a, in order to stop the ongoing reaction before transferring the material sample to another device or container. The sample can also be diluted before subsequent removal from the sample capture pocket. Such operating variations are described in more detail below.
    [0072] [0072] Parts of another illustrative embodiment of a sampling device 150 of the present invention are shown in figures 6a to 8. This sampling device modality 150 is similar to the automatic sampling device 5 described above, but has a smaller number of components individual. In particular, in the alternative embodiment, the inner and outer sleeves 40, 30 and adapter 25 of the previously described embodiment are combined into a single end cap / sleeve element 155 (hereinafter "end cap").
    [0073] [0073] In this embodiment, a proximal part 155a of the end cap 155 is provided with external threads 160 that engage the internal threads 225 of an outer tube 220. The proximal part 155a of end cap 155 has a smaller diameter than a part distal 155b, which results in the formation of a shoulder 165 slightly distal from the end cap threads 160. When the end cap 155 is screwed onto the outer tube 220, the shoulder 160 is brought into contact with the distal end of the outer tube 220 and the end cap is thus attached to it. The proximal part 155a of the end cap 155 also extends into the interior of the outer tube 220 and can produce a sealing contact.
    [0074] [0074] The external tube 220 can be constructed from various materials depending on the substances to which it can be exposed. In this particular embodiment, the outer tube 220 is again constructed of a HASTELLOY material in a similar way to the outer tube 10 of the automatic sampling device 5 of figures 1 to 5.
    [0075] [0075] The distal part 155b of the end cap 155 is provided with an axial hole 170, the diameter of which can approximate the outside diameter of a sample capture element 175 that will pass through it. Consequently, orifice 170 acts as a reciprocal guide for sample capture element 175. The inner surface of orifice 170 also seals against the outer surface of sample capture element 175.
    [0076] [0076] For this purpose, while the end cap 155 can be constructed from various materials depending on the materials to which it can be exposed, it can be determined that the natural elasticity of PTFE creates a good seal when used to build the end cap. far end. In particular, it has been found that the natural elasticity of PTFE allows a good seal to be created with the inside of the outer tube 220, in addition to a good seal with the outer surface of the sample capture element 175 while still allowing low reciprocating. friction of the sample capture element in hole 170 of end cap 155.
    [0077] [0077] When the end cap 155 is made of PTFE or similar material, the hole can be made smaller than the outside diameter of a sample capture element 175 so that when two components are fitted together the TEFLON deforms in the internal orifice and burnishes during installation. Preferably, the size of the hole in the end cap 155 is selected to provide a compressive sealing force against the sample capture element 175.
    [0078] [0078] For operations at higher temperatures, the end cap 155 can be fitted inside a thin metallic sleeve (for example, HASTELLOY). The sleeve operates to contain the expansion of the end cap 155 resulting from higher temperatures, thus maintaining the sealing capabilities of the end cap by balancing the expansion forces with the increased elasticity of PTFE. This allows sampling device 150 to be used and recycled at elevated temperatures while still maintaining the proper function.
    [0079] [0079] As with the automatic sampling device previously described 5, this sampling device 150 also includes a sample capture element 175. As described, and better illustrated in figure 7, sample capture element 175 is located for reciprocate within orifice 170 of end cap 155. For that purpose, the outside diameter of sample capture element 175 is close in dimension to the inner diameter of orifice 170 in end cap 155, so that a tight fit, but slidingly oriented is produced between them (as described above).
    [0080] [0080] The length of the sample capture element 175 may vary depending on the length of the outer tube 220 and / or other components of the sampling device 150. The length of the sample capture element 175 is at least sufficient to extend beyond the end proximal 155a of end cap 155 for a distance that is minimally equivalent to the desired sample capture element extension length.
    [0081] [0081] As more clearly illustrated in figures 7 and 8, the sample capture element 175 of this embodiment includes an elongated cylindrical body with an externally screwed proximal end 175a. As can be seen in figure 7, the screwed proximal end 175a of the sample capture element 175 is received within a similar screwed distal end 230b of a substantially hollow inner tube 230 which is concentricly disposed within the outer tube 220. A collar 180 with increased diameter, it can surround the outside of the sample capture element 175 distally from the threads in order to support the inner tube 230 and allow the secure threaded installation of the sample capture element 175. As with the sampling device automatic previously described 5, the proximal end 230a of the inner tube 230 extends through the proximal end 220a of the outer tube 220 and can be similarly connected to a trigger (not shown) that provides the desired extension and retraction of the capture element sample 175.
    [0082] [0082] The sample capture element 175 of this modality can be constructed from a HASTELLOY material, as described above, but it can also be constructed from various other materials depending on the substances to which it will be exposed and provided that the desired fit between the elements of cooperation are preserved. For example, sample capture element 175 can also be constructed from certain ceramic materials.
    [0083] [0083] With reference to figure 7, it can be seen that when the sample capture element 175 is in a retracted position, a space 235 exists between the collar 180 of the sample capture element 175 and the proximal end 155a of the cap. end 155. The length of this space 235 again represents the maximum possible extension length of the sample capture element 175, since, as illustrated in figure 7, the contact between the collar 180 and the proximal end 155a of the end cap 155 will function as a hard stop with respect to the extension of the sample capture element 175. An associated driver can also have a pitch that is less than the gap 235, in which case the contact between the collar 180 and the proximal end 155a of the end cap 155 may not occur.
    [0084] [0084] During the extension and retraction of the sample capture element 175, the sample capture element is guided by the contact between its outer surface and the inner surface of the orifice 170 in the end cap 155. The appropriate axial linear movement of the element sample capture 60 is thus guaranteed. Due to the second threaded engagement of the sample capture element 175 and inner tube 230, rotation of the sample capture element 715 is prevented without interfering with the ability of the sample capture element to reciprocate along the longitudinal geometric axis of the sampling device. sampling 150.
    [0085] [0085] When the sample capture element 175 is in a retracted (closed) position, as shown in figures 6a and 7, the distal end 175b is preferably positioned substantially homogeneously with the distal end 155b of the end cap 155. When the sample capture element 175 is in an extended (sampling) position, as shown in figure 6b, the distal end 175b projects from the distal end 155 b of the end cap 155 by some predetermined distance.
    [0086] [0086] As illustrated in figures 6a, 7 and 8, the sample capture element 175 is again provided with a concave sample capture pocket 185 that operates as described above to capture a quantity of a sample in which the distal end of the sampling device 150 is immersed. Sample capture pocket 185 can be supplied in different sizes to capture different sample volumes.
    [0087] [0087] The sample capture element 175 is opened again to allow purging / ventilation and to allow cooling of material samples located in sample capture pocket 185. For this purpose, sample capture pocket 185 is provided with a cooling port 190 and a purge / vent port 195, each of which is associated with a corresponding channel 200, 205 that runs through the sample capture element 175 and exits through the proximal end 175a. Grooves 210, 215 are provided in end cap 155 to allow ports 190, 195 in sample capture pocket 185 to communicate with corresponding channels 200, 205 in sample capture element 175 during a cooling cycle and / or purge / ventilation.
    [0088] [0088] As with the automatic sampling device 5 described above, an override groove 240 can be provided to allow the circulation of a cooling medium while the sample capture element 175 is in an extended position. Also similarly to the automatic sampling device 5 described above, the similar piping or conduit can be connected to each of the cooling and / or purge / ventilation channels 200, 205 to take the cooling materials to the sample capture pocket. 185, and to allow ventilation and allow material to be purged from the sample capture pocket. Such tubing can again be routed through the inner tube 230 and can be connected to the sample capture element 175 as previously described.
    [0089] [0089] The use of sampling device 150 generally occurs in the same way as described above with respect to the automatic sampling device 5 of figures 1 to 5, that is, at least the distal end to end cap 155 is typically immersed on or suspended over a material from which a sample is to be extracted. At the desired moment, the trigger (energized or manually activated) is activated to extend the sample capture element 175. This causes the sample capture element 175 to enter the material to be sampled, where a quantity of material fills the pocket sample capture 185 and remain there as the trigger is subsequently activated to retract the sample capture element back into its closed position.
    [0090] [0090] With the sample of the material trapped in the sample capture pocket 185, the sample can be processed such as, for example, by mixing, diluting or by contact with a cooling substance in order to interrupt an ongoing reaction before transfer of the material sample to another device or container. Such operating variations are described in more detail below.
    [0091] [0091] An alternative illustrative embodiment of a sample capture element 300 and an associated sleeve element 345 are shown in figures 9a and 9b and 10a and 10b. Such a modality can be effective when it is desired or necessary to build a sample capture element from a hard material such as glass or ceramic. While small holes, channels and other accessories of a metallic sample capture element can be created by various techniques, including EDM (electrical discharge machining) techniques, the creation of such small accessories in a sample capture element of glass, ceramics, etc. it can be substantially more difficult, if not impossible. Therefore, it was discovered that with a sample capture element made of such hard materials, the movement of several passages (ducts) of it out of the surface allows the same function to be achieved while simplifying or allowing the necessary machining (or forming ). In addition, the fixation of the pipe or similar conduit can also be moved out of the sample capture element, where there is more space.
    [0092] [0092] The illustrative embodiment of the sample capture element 300 is illustrated in an extended position in figures 9a and 9b and in a retracted position in figures 10a and 10b. Such sample capture element positions will be well understood by virtue of the previously described illustrative embodiments of the present invention.
    [0093] [0093] As illustrated, the sample capture element 300 again includes a concave sample capture pocket 305 which, during the extension of the sample capture element, is exposed to and captures a quantity of a sample in which the distal end of the Sample capture element 300 is immersed. The sample capture pocket 305 can again be supplied in different sizes to capture different sample volumes (aliquots).
    [0094] [0094] The sample capture pocket 305 is provided with a cooling port 310 and a purge / vent port 315 which, when the sample capture element 300 is in a stowed position, are placed in fluid communication with the corresponding conduits 320, 325 which run longitudinally along the outer surface of the sample capture element 300 and exit into the entrance / exit doors 330, 335, near the proximal end 300a thereof. This fluid communication is described in more detail below.
    [0095] [0095] The sample capture element 300 can also be provided with an overflow port 340 that allows the supply and possible circulation of a cooling medium through the ducts 320, 325 while the sample capture element is in an extended position . This cooling medium supply and / or recirculation is described in more detail below.
    [0096] [0096] The sample capture element 300 is illustrated to reside and reciprocate within a sleeve 345. As described above with respect to the illustrative modalities described previously, sleeve 345 can again be manufactured from a PTFE material, such as TEFLON . The use of other sleeve materials may also be possible depending on the particular material from which the sample capture element 300 is constructed. The outer diameter of the sample capture element 300 and the inner diameter of the sleeve 345 have a dimension that produces a sealed but slidably oriented fit between them, so that there is no leakage of fluid from the capture element ducts. of sample 320, 325.
    [0097] [0097] As can be better seen in figures 9b and 10b, sleeve 345 is provided with a pair of elongated and axially directed transfer ports 350 that pass through the sleeve wall. As described in more detail below, transfer ports 350 allow fluid communication between sample capture element ducts 320, 325, and, depending on the position of sample capture element 300, the overflow port sample capture element 340 or cooling port 310 and purge / vent port 315 in sample capture pocket 305.
    [0098] [0098] The sample capture element 300 is illustrated in an extended position in figures 9a and 9b where the sample capture pocket 305 is exposed for collecting a sample from a volume of material within which the capture pocket of sample would be immersed. As can be seen more clearly in Figure 9b, in that position, an arcuate section of each sample capture element 320, 325 is placed in fluid communication with a first end of the transfer ports 350 of the sleeve 345. Simultaneously, the The second end of each transfer port 350 is placed in fluid communication with the overflow port 340 on the sample capture element 300. Consequently, when the sample capture element 300 is in an extended position, a cooling medium can be used. supplied and stored or can be recirculated through a fluid path defined by the inlet and outlet ports 330, 335, the ducts 320, 325, the transfer ports 350, and the overflow port 340. The supply of cooling medium for one sample capture element in this way has been generally explained above and therefore need not be mentioned again here.
    [0099] [0099] The sample capture element 300 is illustrated in a retracted position in figures 10a and 10b, where the sample capture pocket 305 is removed into the sleeve 345 to allow action on a trapped material sample. As can be seen more clearly in Figure 10b, when the sample capture element 300 is in the stowed position, the arcuate section of each sample capture element pipeline 320, 325 is placed in fluid communication with the second end of the sleeve transfer ports 350. Simultaneously with this, the first ends of the transfer ports 350 are respectively placed in fluid communication with the cooling port 310 and the vent / vent port 315 in the sample capture pocket 305. Consequently , when the sample capture element 300 is in a retracted position, a sample in the sample capture pocket 305 can be cooled, diluted and removed to another container or device, and the sample capture pocket can be purged with a gas or other fluid, through a fluid path defined by inlet and outlet ports 330, 335, conduits 320, 325, transfer ports 350, and the resf port 310 and purge / vent port 315. Operational variations are described in more detail below.
    [0100] [00100] When using any of the illustrative modalities described above for a sampling device of the present invention, the sampling device can be readied for sampling, such as first by cleaning sampling lines (tubing) by purging with neutral fluids, gases or an inert gas. It is also possible to remove a vacuum before purging the sampling lines. Such cleaning can be carried out cyclically to ensure that any impurities are removed. Depending on the design of the sampling device, the cooling / dilution lines can be pre-filled with the respective fluids.
    [0101] [00101] At a suitable time, the sample capture element is extended and an aliquot of the reaction mixture is captured by the sample capture pocket. Depending on the material (for example, the reaction mixture) being sampled, actual sampling can take place immediately after the sample capture element is extended or with a certain period of time thereafter, so that the sample capture pocket can be purged with the reaction mixture before taking a sample.
    [0102] [00102] With a sample of the material in the sample capture pocket, the sample capture element is then retracted, trapping the material sample in the sample capture pocket and making it available for immediate processing. Depending on the scheme desired by a user of the sampling device, several actions can occur subsequently. First, the sample of material can be contacted with a cooling fluid, whereby the reaction is stopped very quickly, if not immediately. In this case, the material sample represents the reaction mixture substantially as it existed at the time of sampling. The cooled sample can then be diluted and discharged to a respective analyzer, such as, for example, a gas chromatograph, an HPLC, a combination of both, or one or more other suitable analyzers. Under an alternative scheme, the sample can be diluted only, and discharged (for example, sent to an analyzer) as it is without first being cooled. Under another scheme, the sample is diluted before being cooled. While this technique may be less efficient, it may be necessary, for example, in a case where the cooling material cannot be dissolved in the solvent used for the reaction. As a specific example, it would be possible to take a sample from a biological reaction and use a cooling material that is soluble only in a toxic solvent. The cooling and dilution steps can also be combined in other ways not specifically described here.
    [0103] [00103] The dilution and discharge steps of a material sample can be performed in several ways. For example, a continuous stream of fluid (for example, a suitable solvent or gas) can be used, which stream distributes the material sample to the analyzer. Alternatively, a specified amount of dilution fluid can be pumped cyclically through a concentrated sample and then used for sample discharge. In this technique, the sample will be thoroughly mixed with the dilution fluid. Such a technique may be desirable or necessary, for example, when sampling paste reaction mixtures. It may also be possible to use a vacuum pump to discharge a cooled, diluted or unmodified sample of material.
    [0104] [00104] An illustrative (manual) hand-operated sampling device 400 of the present invention is illustrated in figures 11 and 12. Similar to the previously described sampling devices 5, 150, this manual sampling device 400 also includes a set of sample capture 405 which includes an outer tube 410 within which a reciprocating sample capture element 415 is arranged. While sample capture set 405 is illustrated here as being similar in construction to sample capture set 20 of the illustrative embodiment illustrated in figure 1, it should be understood that a manual sampling device of the present invention can also employ a sample capture set of the drawing described with respect to the sampling device 150, or of a drawing not specifically illustrated and described here.
    [0105] [00105] This manual sampling device 400 also includes a body part 420 that houses a probe driver assembly of which only a lever 425 is visible. As indicated by the arrows, lever 425 is rotatable between an extended position (as illustrated) and a position in which the lever is substantially pressed against the body part 420 of the device 400. In this particular example, an internal movement of lever 425 produces an extension of the shape capture element 415. After the release of lever 425, a spring or similar mechanism retracts the shape capture element 415 back into the outer tube 410 and returns lever 425 to its illustrated extended position . Such a mechanism should be well known to those skilled in the art and is therefore not described in further detail here.
    [0106] [00106] In an alternative embodiment of a manual sampling device (not shown), the reciprocating of the sample capture element can be performed by the user triggering a linear plunger set, such as one or more commonly found plunger sets in commercially available pipettes that would be familiar to those skilled in the art.
    [0107] [00107] The body part 420 of this modality, in addition to the body parts of other modalities of a manual sampling device of the present invention, can be provided with a handle 430 or other accessories that facilitate grabbing and / or manipulation by a user . The body part of a manual sampling device of the present invention can also be shaped or contoured to facilitate grabbing and / or manipulation by a user.
    [0108] [00108] As illustrated, sampling lines 435 project from manual sampling device 400. As can be understood from the above descriptions of other sampling device modalities 5, 150, such sampling lines 435 are provided for supply processing materials (eg, cooling or dilution medium) to the sample capture pocket of sample capture element 415, and to carry purged materials away from the sample capture pocket.
    [0109] [00109] For this purpose, the supply sample line 435a is shown in figure 12 as being connected to a processing material supply device 440. In this particular example, the processing material supply device 440 is illustrated as a manually operated syringe that can be used to transfer cooling material, dilution or other sample materials to the sample capture pocket of device 400 to process a sample of material trapped there. In other embodiments, the syringe can be replaced by another device that is operated manually or with an electrical and possibly automated device, such as a pump.
    [0110] [00110] A purge sample line 435b is shown in figure 12 as being connected to a container 445 for receiving the purge material from the sample capture pocket of sampling device 400. The container can simply be a container or it may be a receptacle or other receiving element of an analyzer, such as one or more analyzers described above.
    [0111] [00111] While the structure of this manual sampling device 400 differs from the structure of the automatic sampling device 5 illustrated in figure 5, the function is still substantially the same. That is, the sample capture element is still extended into a sample of interest at an appropriate time and a sample rate is captured by the sample capture pocket. With a sample of the material in the sample capture pocket, the sample capture element is then retracted, trapping the material sample in the sample capture pocket and making it available for immediate processing, as described above. Thus, the primary difference between the automatic sampling device and a manual sampling device of the present invention is simply the fact that the sample capture element of an automatic sampling mode is extended / retracted by an electric actuator (for example, a pneumatic cylinder) or by an electric linear actuator, while the sample capture element of a manual sampling mode is extended and retracted by actuating the operator of a manual actuator (for example, a lever mechanism or linear plunger assembly) .
    [0112] [00112] A specific illustrative method of capturing, processing and discharging a sample of material using the automatic sampling device of the present invention is illustrated in a diagrammatic manner in figure 13. In this particular example, a purge command is sent to the automatic sampling device 500 by a controller communicating with it. Once this purge command is received, the sampling lines of the automatic sampling device are purged with a suitable purge material 405, such as a neutral gas or liquid recovered from a source. The status of the purge operation can be monitored 510. In some cases, this purge step can be skipped during the process of acquiring a material sample.
    [0113] [00113] Once the purging operation has been completed, or in cases where no purging operation is practiced, a probe extension command can be sent 515 to the automatic sampling device, which causes the capture element to sample extends from the outer tube and the sample capture pocket is exposed to the material of interest 520, as described above. The extent of the sample capture element can be monitored 525 to ensure that the sample pocket is fully exposed to the material to be sampled.
    [0114] [00114] In this particular example of the automatic sampling device operation, the captured sample of the material will be cooled. Consequently, once the sample capture element has been properly extended, a capture preparation command can be sent 530 to the automatic sampling device. In this example, this causes the cooling fluid to be pumped into the sampling lines 535 of the automatic sampling device through the overflow port on the sample capture element. In other examples, where an overtaking port is not present, this cooling step can be delayed until after a sample of material has been captured and the sample capture element has been retracted. The filling / circulation of the sampling lines of the automatic sampling device with the cooling fluid can be monitored 540 to ensure that the cooling fluid is available to mix with a captured sample of material.
    [0115] [00115] Since the cooling fluid pumping operation is considered acceptable, or in cases where a cooling fluid pumping operation is delayed (as described above) or where no cooling fluid pumping operation is practiced , a sample capture command can be sent 545 to the automatic sampling device. This causes the sample capture element of the automatic sampling device to retract 550 into the outer tube, trapping a sample of material in the sample capture pocket of the sample capture element and causing the material sample to be cooled. in situ by the cooling fluid residing in the sample capture element.
    [0116] [00116] A selected acquisition command can be subsequently sent 555 to the automatic sampling device. This causes the material sample in the sample capture pocket to be acquired (for example, sent to a suitable analyzer). In this particular example, the acquisition can be made 560 by cyclically pumping a dilution fluid through the material into the sample capture pocket and then discharging the material sample to its next destination, or by using a continuous fluid stream to dilute and discharge the material sample to its next destination. Other dilution / discharge methods and combinations of methods are also possible, as previously described here.
    [0117] [00117] The sample acquisition process can be monitored by finalizing 565. Once the sample acquisition is considered completed, the operation can return to the purge stage 500, or it can wait for the next capture element extension command sample if it is desired to skip the purge step or when no purge step is used.
    [0118] [00118] An illustrative method of capturing, processing, and unloading a sample of material using the manual sampling device of figures 11 and 12 is diagrammatically illustrated in figure 14. In this particular example, the sampling lines of the manual sampling device 605 can be purged with a suitable purging material, such as a neutral gas or liquid, pumped through it by the proper operation 600 of syringe 440. In some cases, this purging step can be skipped during the process of acquiring a sample of material.
    [0119] [00119] Once the purge operation has been completed, or in cases where no purge operation is performed, lever 425 of sampling device 400 is pressed, which causes the sample capture element to extend from the tube outer pocket and the sample capture pocket is exposed to the material of interest 620, as described above.
    [0120] [00120] In this particular example of the sampling device operation, the captured sample of the material will be cooled. Consequently, once the sample capture element has been properly extended, a syringe 440 is operated 620 to transfer the cooling fluid under pressure into the sampling lines 635 of the sampling device through the overflow port on the sample element. sample capture. In other examples, where an overflow port is not present, this cooling step can be delayed until after a sample of material has been captured and the sample capture element has been retracted.
    [0121] [00121] Once the coolant transfer operation is considered acceptable, or in cases where a coolant transfer operation is delayed (as described above) or where no coolant transfer operation is practiced, lever 425 of sampling device 400 is released 630. This causes the sampling device of the sampling device to retract 635 into the outer tube, trapping a sample of the material in the sampling pocket of the sampling device. sample and causing the material sample to be cooled in situ by the cooling fluid residing in the sample capture element.
    [0122] [00122] With the material sample trapped in the sample capture pocket, a 440 syringe can be used to acquire the sample (for example, to send the sample to a suitable container, such as the container of an analyzer). In this particular example, acquisition is accomplished by operating the 640 syringe to push a dilution fluid through the sample lines and into the material in the sample capture pocket to discharge the material sample to its next 645 destination. alternatively, a pump or similar device can be used to supply a continuous flow of fluid to dilute and discharge the material sample to its next destination. Other dilution and discharge methods and combinations of methods are also possible, as previously described here.
    [0123] [00123] With the current sample acquired 650, the operation can return to the purge stage, or to the next sample capture element extension step if it is desirable to skip the purge step or when no purge step is used .
    [0124] [00124] Although the invention has been described by presenting specific illustrative modalities, it is evident that numerous additional variations can be created based on a knowledge of the present invention, for example, by combining the characteristics of the individual examples of the modalities one with another and / or by the exchange of individual functional units between modalities. List of numerical references in figures 13 and 14: 500: Purge command; 505: Purge: Sampling lines purged with gas or neutral liquid; 510: Purge complete 515: Probe extension command; 520: Probe extended - Sample pocket opened for reaction; 525: Probe head extended 530: Capture preparation command; 535: Cooling fluid pumped into the sample lines through the overflow port on the sample head; 540: Cooling on sample lines 545: Sample capture command; 550: Cooling of captured sample retracted in probe 555: Acquisition commands; 560: Sample acquisition - Cyclic pumping then flushing or pumping through the flush; 565: Sample acquired; 600: Operate syringe filled with purging material; 605: Purge - sampling lines purged with gas or neutral liquid; 610: Press the sampling device lever; 615: Probe extended - Sample pocket opened for reaction; 620: Operate a syringe filled with cooling material; 625: Cooling fluid pumped into the sample lines through the overflow port on the sample head; 630: Release the sampling device lever; 635: Cooling of captured sample retracted in the probe; 640: Operate a syringe filled with dilution fluid; 645: Sample acquisition pump then discharges or pumps through discharge; 650: Sample acquired.
    权利要求:
    Claims (17)
    [0001]
    Method of capturing a sample of a material of interest, said method characterized by comprising: providing a sampling device (5, 150, 400), said sampling device (5, 150, 400) including a reciprocating sample capture element (60, 175, 300, 415) located inside an external tube (10, 220, 410) and adapted for extension and retraction with respect to it; a sample capture pocket (65, 305) located near a distal end of said sample capture element (60b), said sample capture pocket (35, 305) adapted to capture a volume of material and having a processing material receiving port (70, 190, 310) and a material expelling port (75, 195, 315) therein; said ports in communication with corresponding channels (80, 85, 200, 2005) in said sample capture element when said sample capture element (60, 175, 300, 415) is in a retracted position; and the sampling lines (435) leading from said channels in said sample capture element (60, 175, 300, 415); positioning a sampling end of said sampling device (5, 150, 400) at or near a sample of a material of interest; causing said sample capture element (60, 175, 300, 415) to extend said sampling device (5, 150, 400) from said outer tube (10, 220, 410) into said sample material interest, thus filling said sample capture pocket (65, 305) in said sample capture element (60, 175, 300, 415) with a quantity of said material; cause said sample capture element (60, 175, 300, 415) to retract from said sampling device (5, 150, 400) into said outer tube (10, 220, 410), thereby trapping a sample of said material of interest in said sample capture pocket (65, 305); processing said material sample in situ within said sample capture pocket (65, 305); and unloading said material sample from said sample capture pocket (65, 305) to a downstream location.
    [0002]
    Method according to claim 1, characterized in that it further comprises purging said sample lines (435) and said sample capture pocket (65, 305) before extending said sample capture element (60, 175 , 300, 415) into a material of interest.
    [0003]
    Method according to claim 1 or 2, characterized in that the processing of said sample of material trapped in said sample capture pocket (65, 305) includes cooling said sample by passing a cooling fluid to it through said processing material receiving door (70, 190, 310).
    [0004]
    Method according to any one of claims 1 to 3, characterized in that the processing of said sample of material trapped in said sample capture pocket (65, 305) includes diluting said sample by passing a dilution material through said processing material receiving door (70, 190, 310).
    [0005]
    Method according to claim 4, characterized in that a specified amount of dilution material is cyclically pumped through said material sample prior to the discharge of said material sample by a dilution material.
    [0006]
    Method according to claim 4, characterized in that a continuous flow of dilution material is used to dilute and discharge said material sample.
    [0007]
    Method according to any one of claims 4 to 6, characterized in that said dilution material is selected from the group consisting of a gas, a liquid solvent, and a neutral liquid.
    [0008]
    Method according to any one of claims 1 to 7, characterized in that it further comprises the passage of a cooling fluid through said sampling lines (435) of said sampling device (5, 150, 400) while said element sample capture (60, 175, 300, 415) is extended into a material of interest.
    [0009]
    Method according to claim 8, characterized in that said cooling fluid is circulated through said sampling lines (435) through an overflow port (340) in said sample capture element (60, 175, 300, 415).
    [0010]
    Method according to any one of claims 1 to 9, characterized in that it further comprises the use of a vacuum pump to discharge or assist in the discharge of said material sample.
    [0011]
    Method according to any one of claims 1 to 10, characterized in that a sample of material is discharged to an analyzer selected from the group consisting of a gas chromatograph, an HPLC device, and a combination thereof.
    [0012]
    Method according to any one of claims 1 to 11, characterized in that said sampling device (5, 150, 400) is an automatic sampling device (5, 150, 400), and where the operational commands are sent to said sampling device (5, 150, 400) automatic by a microprocessor based controller associated with another device used to control or analyze a material of interest.
    [0013]
    Method according to claim 12, characterized in that it additionally comprises monitoring one or more steps of a sample capture operation for completion and waiting for confirmation of completion before proceeding to a subsequent step.
    [0014]
    Method according to any one of claims 1 to 13, characterized in that said sample capture element (60, 175, 300, 415) is extended and retracted by an electric linear actuator (260).
    [0015]
    Method according to any one of claims 1 to 13, characterized in that the sample capture element (60, 175, 300, 415) is manually extended and retracted by a user of said device.
    [0016]
    Method according to any one of claims 1 to 15, characterized in that the method comprises: the provision of said sampling device (5, 150, 400), which is an automatic sampling device (5, 150, 400), said automatic sampling device (5, 150, 400) including said capture element reciprocating sample (60, 175, 300, 415) located inside said external tube (10, 220, 410) and adapted to extend and retract with respect to it; said sample capture pocket (65, 305) located near said distal end of said sample capture element (60, 175, 300, 415), said sample capture pocket (65, 305) adapted to capture a volume of material when extended and to trap said volume of material when retracted, said sample capture pocket (65, 305) having said processing material receiving port (70, 190, 310) and said port expelling material (75, 195, 315), said ports in communication with the corresponding channels in said sample capture element (60, 175, 300, 415) when said sample capture element (60, 175, 300, 415) is in a stowed position, and the sampling lines (435) leading from said channels in said sample capture element (60, 175, 300, 415); connecting said automatic sampling device (5, 150, 400) to a driver (260) adapted to produce a selective tension and retraction of said sample capture element (60, 175, 300, 415); positioning said sampling end of said automatic sampling device (5, 150, 400) on or through a sample of a material of interest; activating said trigger to cause said sample capture element (60, 175, 300, 415) of said automatic sampling device (5, 150, 400) to extend from said external tube (10, 220 , 410) into said material of interest, thus filling said sample capture pocket (65, 305) in said sample capture element (60, 175, 300, 415) with an amount of said material; activating said trigger to cause said sample capture element (60, 175, 300, 415) of said automatic sampling device (5, 150, 400) to retract into said external tube (10, 220 , 410), thus trapping a sample of said material of interest in said sample capture pocket (65, 305); processing said material sample in said sample capture pocket (65, 305) by passing processing material through said sampling line (435) to said corresponding channel in said sample capture element (60, 175, 300, 415), and said processing material receiving door (70, 190, 310) in said sample capture pocket (65, 305); and unloading said material sample from said sample capture pocket (65, 305) to a downstream location through said expulsion port in said sample capture pocket (65, 305), to said corresponding channel in said sample capture element (60, 175, 300, 415), and said sample line (435) connected thereto.
    [0017]
    Sampling device (5, 150, 400) for capturing a sample of a material of interest according to the method as defined in any one of claims 1 to 16, said device characterized by comprising: a reciprocating sample capture element (60, 75, 300, 415) located inside an external tube (10, 220, 410) and adapted to extend and retract with respect to it; a sample capture pocket (65, 305) located near a distal end of said sample capture element (60b), said sample capture pocket (65, 305) adapted to capture a volume of material; a receiving port for processing material (70, 190, 310) located in said sample capture pocket (65, 305); a material expulsion port (75, 195, 315) located in said sample capture pocket (65, 305); corresponding channels in said sample capture element (60, 175, 300, 415), said channels in communication with said ports when said sample capture element (60, 175, 300, 415) is in a retracted position ; a sampling line (435) leading from a channel in said sample capture element (60, 175, 300, 415) to at least one supply of processing material to supply the processing material to said sample capture pocket (65, 305) for in situ processing of a sample of material; and a sampling line (435) leading from a channel in said sample capture element (60, 175, 300, 415) to at least one downstream container for receiving material expelled from said sample capture pocket (65, 305).
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    TW542729B|2003-07-21|Prefilled device
    同族专利:
    公开号 | 公开日
    KR20130131287A|2013-12-03|
    EP2585218B1|2017-07-19|
    EP2585218A1|2013-05-01|
    JP2013535011A|2013-09-09|
    WO2011161111A1|2011-12-29|
    US20130074581A1|2013-03-28|
    US8789431B2|2014-07-29|
    CN102958613B|2015-04-01|
    US8312780B2|2012-11-20|
    CN102958613A|2013-03-06|
    US20110314900A1|2011-12-29|
    BR112012032727A2|2016-11-29|
    JP5749801B2|2015-07-15|
    KR101856796B1|2018-05-10|
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    法律状态:
    2018-02-20| B25D| Requested change of name of applicant approved|Owner name: METTLER-TOLEDO GMBH (CH) |
    2018-03-06| B25H| Request for change of headquarter rejected|Owner name: METTLER-TOLEDO GMBH (CH) |
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2019-03-12| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|
    2019-12-24| B06A| Patent application procedure suspended [chapter 6.1 patent gazette]|
    2020-05-05| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-06-30| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 21/06/2011, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    US12/823,718|2010-06-25|
    US12/823,718|US8312780B2|2010-06-25|2010-06-25|Sampling device and method|
    PCT/EP2011/060364|WO2011161111A1|2010-06-25|2011-06-21|Sampling device and method|
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