Pressure-stepped chemical reactions and associated methods, systems, apparatuses, and articles

Abstract

To provide pressure-stepped chemical reactions and associated methods, systems, apparatuses, and articles.SOLUTION: In an acid digestion reaction performed in a vessel, an elastic lid or septum can be mounted to the mouth of the vessel with a flanged band. In response to determining that a predetermined pressure has been reached in the vessel, a closing force being applied to the lid or septum can be reduced to initiate venting from the vessel. One or more parameters, including the closing force, can be monitored during the venting, and the closing force can be responsively adjusted to optimize the venting. The closing force can be provided by a clamping apparatus that may or may not include a hydraulic system. The clamping apparatus can be configured to increase the closing force in response to increased hydraulic pressure in the hydraulic system.SELECTED DRAWING: None

Description

Background Art

[0001] Decomposition reactions facilitated using laboratory equipment are typically carried out at high temperatures and high pressures. Such decomposition reactions may be reactions between a sample and a strong acid under high temperature and high pressure. The combination of high temperature and strong acid tends to break most, often all, of the chemical bonds within the sample, producing a liquid containing the constituent species of the sample, usually elements. Subsequently, the liquid can be analyzed to examine the presence and quantity of these elements.

[0002] Microwave systems are often used to accelerate the decomposition reaction process. Since microwaves usually interact directly with the decomposition acid and the sample composition, decomposition can be carried out more rapidly than with conventional heat sources.

[0003] Decomposition can be carried out using several different acids (e.g., sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, hydrofluoric acid, perchloric acid, etc.), but nitric acid is advantageous in some situations. In particular, nitric acid usually avoids the formation of insoluble compounds with many inorganic samples. Other acids (e.g., sulfuric acid and hydrochloric acid) are more likely to form such insoluble compounds during the decomposition reaction. Therefore, nitric acid is often used for decomposition to produce high-quality samples for analytical testing.

[0004] To carry out decomposition in nitric acid, some samples need to be heated above the atmospheric boiling point of the acid. At typical atmospheric pressure, nitric acid (e.g., a typical nitric acid solution) boils at about 120°C, but many samples do not decompose completely unless heated to at least about 200°C, and some samples require temperatures of 270 - 300°C. Therefore, to reach higher temperatures, nitric acid decomposition is often carried out in a pressurized environment, usually using a reaction vessel that can withstand pressures of hundreds of pounds per square inch.

[0005] To prevent catastrophic failures at such pressures, the decomposition vessel may include or be associated with a pressure relief mechanism. Such a pressure relief mechanism is known to periodically release pressure by venting the vessel's headspace during decomposition. When releasing pressure, it is usually desirable to vent only the gas in the vessel's headspace so as not to release any analyte. However, a rapid pressure drop in the vessel during venting may cause some of the analyte to be unintentionally discharged from the vessel and / or other problems may occur. [Overview of the Initiative] [Means for solving the problem]

[0006] One aspect of the present disclosure provides a closure (e.g., a lid, cap, cap assembly, partition, etc.) configured to be removably attached to an opening defined by the mouth of a reaction vessel, the closure can be used to provide both a closed and a ventilated configuration of the vessel, and the closure can be configured and operated to ensure that only gas is discharged from the headspace of the vessel during a ventilated configuration (e.g., a configuration that typically does not discharge analytes from the vessel), as will be further described below. The closure may be a lid (e.g., an elastic partition) or include such a lid.

[0007] The closure may optionally further include a band or other suitable structure configured to removably attach the lid to the container. The band may include a body extending at least partially around a hole and defining the hole, and a plurality of latches (e.g., at least two latches) extending downward from the body and configured to removably attach the band and the lid to the container by elastically deforming and releasably engaging with a predetermined portion of the container (e.g., a flange). The plurality of latches may be configured to extend at least partially collectively around the container. In one example (e.g., optionally), gas to be vented out of the container may pass through one or more openings defined between adjacent latches.

[0008] Another aspect of the present disclosure is to provide a method for controlling pressure and preserving analytes in an acid digestion reaction carried out at high temperature and high pressure. The method may include providing a sealed closure configuration for a reaction vessel while the reaction vessel contains reactants, including the acid and the sample. Providing a sealed closure configuration may include increasing a closing force (e.g., a clamp) that holds an occlusion (e.g., a lid or elastic stub) against the mouth of the reaction vessel, and stopping the increase in the closing force in response to determining from at least one signal that a predetermined closing force has been reached. The reactants in the reaction vessel may be heated (e.g., by microwaves) during the sealed closure configuration, thereby increasing the pressure inside the reaction vessel. In response to determining that a predetermined pressure has been reached inside the reaction vessel, the closing force may be reduced to initiate ventilation from the reaction vessel to the outside. During ventilation, the pressure inside the reaction vessel may be monitored, and the closing force may be adjusted to ensure that only gases from the headspace of the reaction vessel are vented (e.g., typically without venting any analytes from the reaction vessel).

[0009] A further aspect of the present disclosure is to provide a system for carrying out a decomposition reaction. The system may include a support configured to support a reaction vessel; a clamping device configured to apply a closing force toward the mouth of the reaction vessel while the reaction vessel is supported by the support; a heating device configured to heat the contents of the reaction vessel (e.g., by microwaves) while the reaction vessel is supported by the support; a first sensor configured to provide a signal indicating the gas pressure in the headspace of the reaction vessel while the reaction vessel is supported by the support; a second sensor configured to provide a signal indicating the closing force; and a computer configured to control the closing force and ventilation to the outside from the opening of the reaction vessel via the clamping device in response to an input while the reaction vessel is supported by the support. The input may include one or more signals from the first sensor and the second sensor.

[0010] As an example, a clamping device may include a hydraulic system and an actuator (e.g., a motor) configured to operate in a manner that increases the hydraulic pressure within the hydraulic system. The clamping device may be configured to increase the closing force in response to an increase in the hydraulic pressure within the hydraulic system. Alternatively, the hydraulic mechanism may be omitted from the clamping device.

[0011] The clamping device may include an engager, and the clamping device may be configured to clamp at least a portion of the closure (e.g., an elastic partition) between the underside of the engager and the mouth of the reaction vessel. The underside of the engager may include an upward-extending recess that extends at least partially around a downward-projecting portion of the engager. The upward-extending recess may be configured to adapt to the upward movement of a portion of the closure in an attempt to improve the accuracy of the signal from the first sensor.

[0012] According to another aspect of the present disclosure, a support configured to support a reaction vessel may include a frustoconical surface configured to engage with the corresponding frustoconical outer surface of the reaction vessel.

[0013] The above overview provides some brief examples and is not exhaustive; the present invention is not limited to these examples. The aforementioned examples and other examples will be further described in the following detailed description with reference to the accompanying drawings. The present invention provides, for example, the following: (Item 1) A cap assembly configured to be removably attached to the opening defined by the mouth of a reaction vessel, the cap assembly is: They are a band, A body that extends at least partially around the hole and defines the hole, A plurality of latches extending downward from the main body, configured to removably attach the band to the mouth of the reaction vessel by elastically deforming and removably engaging with a predetermined portion of the reaction vessel, and A band equipped with, A lid configured to simultaneously close both the hole in the main body and the opening of the reaction vessel. Equipped with, A cap assembly in which the plurality of latches are configured to extend collectively, at least partially, around the reaction vessel. (Item 2) The cap assembly described above, wherein the lid has a lateral dimension smaller than the gap defined between opposing latches such that the plurality of latches collectively extend at least partially around the lid. (Item 3) The cap assembly according to any one of the above items, wherein the above lateral dimension of the lid is the diameter of the lid. (Item 4) The above gap is the first gap between the opposing latches, The cap assembly according to any one of the above items, wherein the above lateral dimension of the above lid is greater than the second gap defined between the opposing latches. (Item 5) The cap assembly according to any one of the above items, wherein the second gap is defined between the tabs extending inward from the opposing latches. (Item 6) The cap assembly according to any one of the above items, wherein each of at least some of the latches is configured to engage releasably below the rim of the mouth of the reaction vessel. (Item 7) For each of at least some of the above-mentioned latches, the latch includes a tab that is spaced apart from the band and extends below the cover. The cap assembly according to any one of the above items, wherein the edge of the lid is engaged with and supported by the tab. (Item 8) A cap assembly according to any one of the above items, wherein an opening is defined between adjacent latches among the above-mentioned multiple adjacent latches. (Item 9) A cap assembly according to any one of the above items, wherein a gap is defined between adjacent latches among the multiple adjacent latches described above. (Item 10) A cap assembly according to any one of the above items, wherein multiple gaps are defined between adjacent latches among the multiple adjacent latches described above. (Item 11) The cap assembly according to any one of the above items, wherein the lid is provided with a partition, the partition being a sheet at least partially formed of a fluoropolymer that is inert to mineral acids. (Item 12) A method for controlling pressure and preserving an analyte in an acid digestion reaction carried out at least partially at a temperature and pressure exceeding ambient temperature and ambient pressure, the method being: While the reaction vessel contains reactants including an acid and a sample, providing a sealed closed configuration for the reaction vessel, the provision of the sealed closed configuration comprising increasing a closing force that holds a closure against the mouth of the reaction vessel and stopping the increase in the closing force in response to determining from at least one signal that the closing force has reached a predetermined closing force, heating the reactants in the reaction vessel within the sealed closed configuration such that the pressure within the reaction vessel increases, venting to the outside through the opening in response to determining from at least one signal that a predetermined pressure has been reached within the reaction vessel, the venting to the outside comprising reducing the closing force, A method comprising. (Item 13) The method according to the above item, comprising determining the pressure within the reaction vessel from at least one signal during the venting. (Item 14) During the venting, determining a change in pressure within the reaction vessel from at least one signal, and adjusting the closing force in response to the determined change in pressure within the reaction vessel that varies from a predetermined change in pressure. The method according to any one of the above items, comprising. (Item 15) The method according to any one of the above items, wherein the closure comprises an elastic diaphragm. (Item 16) The method according to any one of the above items, wherein the predetermined pressure within the reaction vessel is the gas pressure within the headspace of the reaction vessel. (Item 17) The method according to any one of the above items, wherein the heating of the reactants comprises directing microwave energy towards the reactants and the microwave energy passing through at least one side wall of the reaction vessel. (Item 18) The method according to any one of the above items, comprising stopping the heating in response to a determination that the predetermined pressure has been reached within the reaction vessel. (Item 19) The increase in the closing force is configured to increase the hydraulic pressure in response to the operation of the motor, The method according to any one of the above items, wherein the increase in the closing force responds to the increase in the hydraulic pressure. (Item 20) The venting essentially consists of venting gas from the headspace in the reaction vessel to the outside, the method according to any one of the above items. (Item 21) At least one vent passage is defined in response to the decrease in the closing force, The method according to any one of the above items, wherein at least a part of the vent passage is defined by a gap positioned between the closure and the mouth of the reaction vessel. (Item 22) The closure includes a flexible partition removably attached to the mouth of the reaction vessel via at least a plurality of latches, The method according to any one of the above items, wherein a part of the vent passage extends between the latches of the plurality of latches. (Item 23) The predetermined closing force is the first closing force, and the predetermined pressure is the first pressure, After the venting and before removing the reaction vessel from the instrument on which the method is performed, sealing the reaction vessel with a second closing force greater than the first closing force, and then venting to the outside from the opening in response to a second pressure in the reaction vessel greater than the first pressure, The method according to any one of the above items, further comprising. (Item 24) The sealed closing configuration is the first sealed closing configuration, the predetermined closing force is the first predetermined closing force, the predetermined pressure is the first predetermined pressure, and the method is, The present invention provides a second sealed closure configuration for the reaction vessel while the reaction vessel contains at least a portion of the reactants, wherein the provision of the second sealed closure configuration comprises increasing the closure force until it is determined from at least one signal that a second predetermined closure force is reached, and the second predetermined closure force is greater than the first predetermined closure force. Further heating of at least a portion of the reactants in the reaction vessel within the second sealed closed configuration so as to further increase the pressure inside the reaction vessel, Venting air outward through the opening in response to determining from at least one signal that a second predetermined pressure has been reached in the reaction vessel, wherein the second predetermined pressure is greater than the first predetermined pressure. The method described in any one of the above items, further including: (Item 25) A system for carrying out a decomposition reaction, the system is A support configured to support the reaction vessel, A clamping device configured to apply a closing force toward the mouth of the reaction vessel while the reaction vessel is supported by the support, A heating device configured to heat the contents of the reaction vessel while the reaction vessel is supported by the support, A first sensor configured to provide a signal indicating the gas pressure in the headspace of the reaction vessel while the reaction vessel is supported by the support, A second sensor configured to provide a signal indicating the closing force, A computer configured to control the closing force and the ventilation outward from the opening of the reaction vessel via the clamping device in response to an input while the reaction vessel is supported by the support, wherein the input includes a signal from the first sensor and a signal from the second sensor, and A system that includes these features. (Item 26) The clamping device includes an engaging portion configured to reciprocate toward and away from the support, and the system is The above reaction vessel and, An elastic partition configured to be clamped between the mouth of the reaction vessel and the engaging portion, The system described in the above items, which includes the above features. (Item 27) It is equipped with a band, and the band is A body that extends at least partially around the hole and defines the hole, A plurality of latches extending downward from the main body, configured to removably attach the band and the partition to the opening of the reaction vessel by elastically deforming and removably engaging with a predetermined portion of the reaction vessel, and A system comprising any one of the above items. (Item 28) The clamping device described above comprises a hydraulic system and a motor configured to operate in such a way as to increase the hydraulic pressure within the hydraulic system. The system according to any one of the above items, wherein the clamping device is configured to increase the closing force in response to an increase in the hydraulic pressure in the hydraulic system. (Item 29) The above support is equipped with a receptacle, The receptacle has a frustoconical inner surface configured to face and make direct contact with the reaction vessel, The frustoconical inner surface has a variable diameter, The system according to any one of the above items, wherein the diameter of the frustoconical inner surface increases in the vertical direction. (Item 30) A system that performs a decomposition reaction, the system is A support configured to support the reaction vessel, A clamping device equipped with an engagementr, The clamping device is configured to clamp at least a portion of the closure between the underside of the engager and the mouth of the reaction vessel while the reaction vessel is supported by the support, The lower side of the engager has an upward-extending recess that extends at least partially around the downward-protruding portion of the engager, a clamping device, A force sensor, which, by cooperatively associating with a downwardly projecting portion of the engager, provides a signal indicating the pressure inside the reaction vessel while at least a portion of the closure is clamped between the underside of the engager and the opening of the reaction vessel. It is equipped with, The upward-extending recess is configured to adapt to the upward movement of a portion of the closure in order to improve the accuracy of the signal from the force sensor, in a system. (Item 31) The system described above, wherein the upward-extending recess is configured to partially adapt to the upward expansion of the closure in order to improve the accuracy of the signal from the force sensor. (Item 32) The above-mentioned engager is a flexible engaging web that is part of the engaging device. The engagement device further comprises a backing structure configured to press the engagement web toward the mouth of the reaction vessel while the reaction vessel is supported by the support, The system according to any one of the above items, wherein the backing structure is more rigid than the engagement web, defines a through-hole, and through the through-hole, the force sensor is associated cooperatively with the downwardly projecting portion of the engagement web, thereby providing a signal indicating the pressure inside the reaction vessel while the portion of the closure is clamped between the underside of the engagement web and the mouth of the reaction vessel. (Item 33) The clamping device described above comprises a hydraulic system and a motor configured to operate in such a way as to increase the hydraulic pressure within the hydraulic system. The system according to any one of the above items, wherein the clamping device is configured to increase the closing force in response to an increase in the hydraulic pressure in the hydraulic system. (Item 34) The above support is equipped with a receptacle, The receptacle has a frustoconical inner surface configured to face and make direct contact with the reaction vessel, The frustoconical inner surface has a variable diameter, The system according to any one of the above items, wherein the diameter of the frustoconical inner surface increases in the vertical direction. (Item 35) A reaction vessel configured to encompass at least partially a chemical reaction, the reaction vessel is A microwave energy-transmitting and at least one side wall extending around the internal space of the reaction vessel, An opening that defines the upper opening to the interior space and It is equipped with, The upper part of at least one side wall is provided with the frustoconical outer surface of the reaction vessel, The frustoconical outer surface has a variable diameter, A reaction vessel in which the diameter of the frustoconical outer surface increases in a direction along the height of the reaction vessel, extending from the lower end of the reaction vessel toward the upper opening of the reaction vessel. (Item 36) The reaction vessel according to the above item, wherein the upper part of the at least one side wall is thicker than the lower part of the at least one side wall. (Item 37) The lower part of at least one of the above-mentioned side walls defines a thickness that extends from the lower part of the inner surface of the reaction vessel to the lower part of the outer surface of the reaction vessel, The upper portion of at least one side wall has a variable thickness extending from the upper part of the inner surface of the reaction vessel to the frustoconical outer surface of the reaction vessel, The upper thickness of the at least one side wall is greater than the lower thickness of the at least one side wall. The reaction vessel according to any one of the above items, wherein the upper thickness of the at least one side wall increases in a direction along the height of the reaction vessel extending from the lower end of the reaction vessel toward the upper opening of the reaction vessel. (Item 38) The upper part of at least one of the above-mentioned side walls extends further outward than the frustoconical outer surface and defines an annular flange positioned above the frustoconical outer surface, The opening described above has an annular, flat upper surface that extends from around the upper opening into the internal space, The reaction vessel described above is microwave energy permeable as a whole, as described in any one of the above items. (Summary) In an acid decomposition reaction carried out in a vessel, an elastic lid or stub can be attached to the mouth of the vessel by a flanged band. In response to the determination that a predetermined pressure has been reached in the vessel, the occluding force applied to the lid or stub can be reduced to initiate ventilation from the vessel. One or more parameters, including the occluding force, can be monitored during ventilation, and the occluding force can be adjusted responsively to optimize ventilation. The occluding force can be provided by a clamping device, which may or may not include a hydraulic system. The clamping device may be configured to increase the occluding force in response to an increase in hydraulic pressure in the hydraulic system. The clamping device may include an enterger having an upward-extending recess that extends at least partially around a downward-projecting portion of the enterger. [Brief explanation of the drawing]

[0014] The drawings are provided as examples. The present invention can be embodied in many different forms and should not be construed as being limited to the examples shown in the drawings.

[0015] [Figure 1] Figure 1 is a high-level diagram of a system used to facilitate a pressure-stepped decomposition reaction according to one embodiment of the present disclosure.

[0016] [Figure 2] Figure 2 is a top view of the reaction vessel of the system shown in Figure 1.

[0017] [Figure 3] Figure 3 is a drawing of the bottom of the container shown in Figure 2.

[0018] [Figure 4] Figure 4 shows the front, back, right, and left elevation views of the top of the container shown in Figure 2, respectively.

[0019] [Figure 5] Figure 5 is a top view of a band of a closure or cap assembly configured to be attached to the upper end of the container shown in Figure 2, according to one embodiment of the present disclosure.

[0020] [Figure 6] Figure 6 is a bottom view of the band shown in Figure 5.

[0021] [Figure 7] Figure 7 shows the front, rear, right, and left elevation views of the cap assembly in an upright, unmounted configuration.

[0022] [Figure 8] Figure 8 shows the front, rear, right, and left elevation views of the cap assembly in an inverted and unmounted configuration.

[0023] [Figure 9] Figure 9 is a top view of the cap assembly attached to the top of the container.

[0024] [Figure 10] Figure 10 is a bottom view of the cap assembly attached to the top of the container.

[0025] [Figure 11]Figure 11 is a schematic top view of a part of the apparatus including the system shown in Figure 1, according to one embodiment of the present disclosure.

[0026] [Figure 12] Figure 12 is a pictorial cross-sectional view of a part of the apparatus in Figure 11, the cross-section being taken substantially along line 12-12 in Figure 11.

[0027] [Figure 13] Figure 13 is similar to Figure 12, except that the plunger device is in a lower position, according to one embodiment of the present disclosure.

[0028] [Figure 14] Figure 14 is a cross-sectional view of a portion of the apparatus in Figure 11, taken substantially along line 14-14 in Figure 11.

[0029] [Figure 15] Figure 15 is a pictorial representation similar to Figure 14.

[0030] [Figure 16] Figure 16 is a schematic cross-sectional view of a portion of the apparatus in Figure 11, taken substantially along line 16-16 in Figure 11.

[0031] [Figure 17] Figure 17 is a cross-sectional view of a portion of the apparatus in Figure 11, taken substantially along line 17-17 in Figure 13.

[0032] [Figure 18] Figure 18 is similar to Figure 13.

[0033] [Figure 19] Figure 19 is similar to Figure 13 and schematically shows that a portion of the cap assembly bulges outward due to the pressure inside the container, and an upward force is applied.

[0034] [Figure 20]Figure 20 is similar to Figure 13 and schematically shows the plunger device / cap assembly in a ventilated configuration, and the ventilation from the container to the outside (e.g., the ventilation gap is exaggerated for illustrative purposes).

[0035] [Figure 21] Figure 21 is an exploded view of some of the components of the plunger, engagement device, and associated housing of the fixture.

[0036] [Figure 22] Figure 22 is a chart showing the operating parameters of an exemplary pressure-stepped chemical reaction with periodic aeration according to one embodiment of the present disclosure.

[0037] [Figure 23] Figure 23 shows a flowchart of a method that can be performed at least partially by the controller of the device in Figure 11, according to one embodiment of the present disclosure. [Modes for carrying out the invention]

[0038] Examples of embodiments are disclosed below. The drawings illustrate examples of embodiments. In other words, examples of embodiments are described with reference to the drawings. However, the present invention can be embodied in many different forms and should not be construed as being limited to the embodiments described herein. For example, features disclosed as part of one embodiment or example can be used in the context of another embodiment or example to give rise to further embodiments or examples. As another example of the breadth of this disclosure, it is within the scope of this disclosure that one or more terms such as “substantially,” “about,” and “approximately” modify the adjectives and adverbs, respectively, in the detailed description sections of this disclosure, as will be described in more detail below.

[0039] Figure 1 schematically shows a system 10 configured to facilitate, for example, a pressure-stepped chemical reaction (e.g., a decomposition reaction) according to one embodiment of the present disclosure. System 10 is first described below at a high level, with a more detailed description following the initial overview.

[0040] In the example shown in Figure 1, the system 10 includes a reaction vessel 12 configured to contain a chemical reaction and a pressure-responsive blockage or closure 14 (e.g., a cap assembly) that closes the upper opening of the reaction vessel. The closure 14 can be removably attached to the reaction vessel 12 and can be operated to completely close the reaction vessel (e.g., a clamp or closed configuration) and to partially open the reaction vessel (e.g., a vented configuration), as further described below. The operation of the closure 14 to transition between the closed and vented configurations can be controlled by a closing or clamping device configured to provide various forces (e.g., a closing force, a clamping force, or a sealing force) between the closure 14 and the reaction vessel 12. In the illustrated embodiment, the system 10 is configured such that (i) a closing (e.g., clamping) force and one or more other factors (e.g., heating of the contents of the container 12) are controlled in a predetermined manner to provide at least partially pressure-stepped chemical reactions (e.g., decomposition reactions) within the container 12, and (ii) the pressure-stepped chemical reactions consist of alternating sets of closing (e.g., hermetically sealed) configurations and ventilated configurations, and feedback (e.g., "closing force feedback") is used to ensure that only gas is discharged from the headspace of the container (e.g., typically without any analytes being discharged from the reaction vessel) during the ventilated configurations, which will be further described below.

[0041] The contents of container 12 are schematically represented by horizontal dashed lines in Figure 1. If the contents or composition in container 12 are for a decomposition reaction, the composition may include at least one analyte-containing sample and at least one concentrated mineral acid. In some situations, robust extraction is the goal, and the composition may include the sample and an organic solvent. To enhance or accelerate the decomposition reaction in container 12, the contents of the container (e.g., a sample containing an aggressive acid such as nitric acid) may be heated by any suitable method (e.g., by heat conduction through the container wall, by radiation passing through the container wall and being absorbed by the contents of the container, and / or dielectric heating). In the illustrated embodiment, container 12 is microwave-transparent, and the contents of the container are heated by absorbing microwaves from at least one microwave radiation source 15 (e.g., a magnetron).

[0042] The clamping device may include at least one actuator 16 (e.g., an electric motor) and one or more linkages 18, 20, 22 positioned between the actuator 16 and the closure 14. The system 10 may provide feedback of the closing (e.g., clamping) force by including one or more sensors 24, 26, 28 and at least one controller 30 (e.g., a computer) configured in cooperation with, for example, the actuator 16 and / or the linkages 18, 20, 22, which will be further described below. The communication paths between the controller 30, the microwave source 15, the actuator 16, and the sensors 24, 26, 28 are schematically shown by dashed lines in Figure 1, as will be further described below.

[0043] The controller 30 is configured to act responsively on the clamping device so that it can provide sufficient downward closing force to the closure 14 during heating of the container contents and before venting from the container, thereby ensuring that the container is hermetically sealed in a closed configuration. In contrast, during the venting process (e.g., throughout the entire venting process), the closing or clamping force applied to the closure 14 by the clamping device can more closely match (e.g., slightly less) the upward opening force applied to the closure by the pressure inside the container 12 to ensure that only the gas in the headspace of the container is vented (e.g., typically without any analytes being vented from the reaction vessel), which will be further described below. The controller 30 can be configured so that throughout each venting process or cycle, the closing force applied by the clamping device decreases in proportion to the decreasing upward opening force applied to the closure by the pressure inside the container 12 to ensure that only the gas in the headspace of the container is vented (e.g., typically without any analytes being vented from the reaction vessel), which will be further described below.

[0044] As will be further described below, various different types of clamping devices configured to provide a closing or clamping force to at least a portion of the closure 14 are within the scope of this disclosure. In the embodiment shown in Figure 1, the intermediate linkage 20 is a hydraulic system or circuit including at least one hydraulic passage 31 that fluidly communicates between at least one of each of a mechanical-hydraulic converter 32 (e.g., a hydraulic drive) and a hydraulic-mechanical converter 34 (e.g., a hydraulic actuator). The converters 32, 34 may be configured as a master cylinder 32 and a slave cylinder 34, and / or may be referred to as a master cylinder 32 and a slave cylinder 34. However, the converters 32, 34 are not limited to master cylinders and slave cylinders. For example, in an alternative embodiment of this disclosure, the mechanical-hydraulic converter 32 could be a hydraulic pump.

[0045] A master cylinder 32, for example, can define a variable hydraulic volume, at least partially defined by a master displacement member 36 (e.g., a piston or other suitable structure) mounted to reciprocate within a master chamber 38 (e.g., a cylinder or annular sleeve) that is in fluid communication with the hydraulic passage 31. Similarly, a slave cylinder 32 (e.g., a response cylinder), for example, can define a variable hydraulic volume, at least partially defined by a slave displacement member 40 (e.g., a piston or other suitable structure) mounted to reciprocate within a slave chamber 40 (e.g., a cylinder or annular sleeve) that is in fluid communication with the hydraulic passage 31.

[0046] The hydraulic fluid in the hydraulic circuit 20 is schematically represented by pointillism in Figure 1. Those skilled in the art will understand that the pressure applied to the hydraulic fluid by the master displacement member 36 is applied similarly everywhere within the hydraulic circuit 20. A hydraulic sensor 24 (e.g., a load cell) configured to provide a signal indicating the pressure (and therefore indirectly the closing force) of the hydraulic fluid can be mounted to close an opening into the interior of the hydraulic passage, or the hydraulic sensor can be associated with the hydraulic circuit 20 in any other suitable way. The hydraulic measurement provided by the pressure sensor 24 can be used (e.g., by the controller 30) to calculate the effective sealing or closing force applied to the closure 14. This closing force data can be called force feedback data used (e.g., by the controller 30) to help dynamically seal / ventilate the vessel 12 based on the pressure inside the reaction vessel 12, as will be further described below. Alternatively, the signal indicating the closing force can also be provided by force sensors (e.g., load cells) associated with each mechanical component of the downstream linkage 22.

[0047] The downstream linkage 22 may be a mechanical linkage configured to transmit a linear downward force from the slave displacement member 40 to the closure 14 on the reaction vessel 12. The force sensor 26 may provide a signal indicating the pressure in the reaction vessel 12 by being associated with (e.g., supported by) the downstream linkage 22 and operably associated with the movable (e.g., flexible) portion of the closure 14, as further described below. The temperature sensor 28 may provide a signal indicating the temperature in the reaction vessel 12 by being associated with the reaction vessel 12 (e.g., the reaction vessel may be within the field of view of the infrared temperature sensor), as further described below.

[0048] In the illustrated embodiment, the hydraulic sensor 24 can provide signals indicating the pressure of the hydraulic fluid, and these signals can be supplied (e.g., feedback) to the controller 30 as part of providing closing force feedback, as will be further described below. In non-hydraulic embodiments, other structures and methods may be associated with providing closing force feedback. For example, the closing force may be provided by a purely mechanical structure including a lead screw, where signals indicating the closing force can be provided by strain sensors associated with each mechanical component, as will be further described below.

[0049] Figures 2-4 show an exemplary container 12. The container 12 may include at least one side wall 44 extending around an upwardly open internal space of the container. The lower part of the container side wall 44 may be cylindrical and may extend upward from the closed lower end of the container 12, which may be shaped like an inverted spherical cap. The inner surface portion 46 of the container side wall 44 may extend downward from the upper opening 48 of the container. The inner surface portion 46 may be cylindrical from the upper opening 48 to the upwardly concave inner surface of the lower end of the container.

[0050] The annular outer surface of the upper portion of the container side wall 44 tapers in a direction along the height of the reaction vessel 12, thereby defining the frustoconical outer surface 50 of the vessel 12. The outer surface of the container side wall 44 extending between the frustoconical surface 50 and the lower end of the vessel can be cylindrical. Therefore, the upper portion of the container side wall 44 defining the frustoconical surface 50 has a greater thickness than the lower portion of the container side wall 44. The lateral dimension or diameter of the frustoconical outer surface 50 increases vertically along the height of the vessel 12.

[0051] The upper end of the container side wall 44 may define an outwardly projecting annular flange 52, and / or the upper end of the container 12 may include an annular flange 52. Referring to Figure 4, the container flange 52 may include an annular (e.g., cylindrical) intermediate outer surface 53 between the annular chamfered upper outer surface 54 and the lower outer surface 55. The upper end of the container may take the form of an annular flat top seat surface 56 that extends inward from the inner edge of the flange top surface 54 and is coaxial with the container opening 48. The opening 48, together with the flange 52 and the seat surface 56, may be called the mouth of the container. The container 12 is typically constructed of a durable material that transmits microwave energy (e.g., quartz, glass, and / or a suitable high-performance polymer material). As an example, the portion of the container 12 below the frustoconical surface 50 may be like the lower portion of a conventional test tube, and / or any other suitable shape.

[0052] Figures 5 and 6 show exemplary bands 57 of a closure 14 (Figures 7 and 8) configured to snap onto the openings 48, 52, and 56 of a container (Figures 2-4). Referring to Figures 7 and 8, the closure 14 may be a cap assembly including a lid 58 (e.g., a partition or other suitable obstruction) used to seal the container opening 48 (Figure 2). The bands 57 may be configured to releasably hold the lid 58 over the container opening 48, as will be further described below.

[0053] Referring to Figures 5 and 6, the band 57 may include an annular flange 59 extending inward from the upper end of the band's annular (e.g., cylindrical) sleeve 60, and a series of flexible latches 61 extending downward from the lower end of the sleeve. The inner edge of the band flange 59 extends around and defines the upper through-hole 62 at the top of the band. The series of flexible latches 61 may be referred to as multiple latches (e.g., two latches, three latches, four latches, and / or more than four latches).

[0054] The upper portion 63 of the band sleeve 60 and band latch 61 may extend from and / or perpendicular to the band flange 59. The free lower end portion of the band latch 61 may be in the form of an inwardly / diagonally extending tab 64. Openings, spaces, or gaps between adjacent band latches 61 may be referred to as band slots 65. One or more of the band slots 65, or possibly each of them, may be omitted and / or replaced by other features. As another example, one or more of the band slots 65, or possibly each of them, may extend to the band flange 59 and / or be of a different shape (e.g., as a slit and / or opening that is not rectangular). A series of band openings or slots 65 may be referred to as multiple openings or slots (e.g., two openings or slots, three openings or slots, four openings or slots, and / or more than four openings or slots). In the orientations shown in Figures 5-7, one or more, or each of, the band openings or slots 65 (e.g., two openings or slots, three openings or slots, four openings or slots, and / or more than four openings or slots) can open downward and thus extend to the lower end of the band sleeve 60.

[0055] Referring to Figure 7, the lid 58 may be a single-layer or multi-layer sheet in the shape of a disc. The lid 58 may have a lateral dimension or diameter that is slightly smaller than the lateral dimension or inner diameter of the band sleeve 60 and larger than the lateral dimension defined between the opposing latch tabs 64, so that the peripheral or outer edge of the lid engages with and supports the upper portion of the inner surface of the latch tabs 64 when the cap assembly 14 is upright. Referring to Figure 8, the band hole 62 may have a lateral dimension or diameter that is smaller than the lateral dimension or diameter of the lid 58, so that when the cap assembly 14 is inverted, the lid engages with and rests on the band flange 59. Figure 8 is schematic because the lid 58 is not visible and is schematically represented by dashed lines.

[0056] The lid 58 may be called a partition (Figure 1) and is formed of a durable (e.g., acid and high temperature resistant) material having sufficient structure and elastic modules for repeated expansion, thereby reasonably and accurately applying force (indicating pressure inside the container 12) toward the force sensor 26. The lid 58 may be in the form of a disc-shaped sheet of an elastic (e.g., flexible) material, such as a polymer material, more specifically, without limitation, a thermoplastic polymer material such as a fluorocarbon solid (e.g., polytetrafluoroethylene or PTFE, commonly known as Teflon®). The lid 58 may be cut (e.g., die-cut or laser-cut) from a sheet of polytetrafluoroethylene (e.g., extruded or otherwise appropriately formed sheet) having a thickness of about 0.030 inches, so that the lid thickness is thought to be about 0.030 inches, and the polytetrafluoroethylene may or may not contain one or more suitable fillers. A lid 58 containing polytetrafluoroethylene (for example, at least partially or fully formed) can be considered to have a thickness of less than about 0.1 inches, less than about 0.075 inches, less than about 0.050 inches, in the range of about 0.1 inches to about 0.010 inches, in the range of about 0.075 inches to about 0.020 inches, in the range of about 0.050 inches to about 0.025 inches, and / or any value or partial range in between.

[0057] Similarly, the band 57 can be formed from a durable material having sufficient structure and elastic module to snap onto the mouths 48, 52, and 56 of the container 12. The band 57 can be formed from, for example, a polymer material, more specifically, a thermoplastic polymer material such as polypropylene, by, for example, injection molding.

[0058] Referring to Figures 9 and 10, the container opening 48 (Figure 2) can be closed, more specifically closed, by relative movement between the container 12 and the cap assembly 14 (for example, as shown in Figure 7), so that the band latch 61 bends outward in response to engaging and fitting with the container flange 52. After the latch tab 64 slides and engages with the intermediate outer surface 53 of the container flange and moves beyond it, the latch tab can elastically return to its original shape, so that the cap assembly 14 is securely and removably attached to the upper end portion of the container 12. When the cap assembly 14 is securely and removably attached to the upper end of the container 12, the relatively narrow annular rim portion of the upper surface of the lid 58 can face and make contact with the lower surface of the band flange 59; the relatively wide annular rim portion of the lower surface of the lid 58 can face and make contact with the upper seat surface 56 of the container (Figure 2); the inner surface of the upper latch portion 63 can face and make contact with the intermediate outer surface 53 of the container flange; and the inner surface of the latch tab 64 can face and make contact with the lower surface 55 of the container flange.

[0059] The cap assembly 14 can be detached from the container 12 (for example, from a secure and detachable attachment to the upper end of the container 12) in response to relative movement between the container 12 and the cap assembly 14 that separates the container 12 from each other. In response to such relative separation movement, the band latch 61 engages with the container flange 52 and bends outward in response to sliding off the container flange 52. After the latch tab 64 slides through the intermediate outer surface 53 of the container flange, the latch tab can elastically return to its original shape so that the lid 58 is held by the band 14 (for example, caught and supported by the latch tab 64) in the configuration shown in Figure 7 and described above.

[0060] The band 57 can function to conveniently facilitate the placement or positioning of the lid 58. However, optionally, the lid 58 may be used without the band 57. Thus, in some embodiments, implementations, and / or methods of this disclosure, the cap or closure 14 may consist only of the lid 58.

[0061] Figure 11 is a top view of the apparatus 66, including system 10 (Figure 1), providing a reference frame for identifying the location of specific components. Figure 11 shows the upper housing portion 67 and the central housing portion 68. The upper housing portion 67 can be moved relative to the central housing portion 68 to open the apparatus 66, allowing access to the reaction vessel 12 (Figures 1-4) supported by the central housing portion, for example, as will be further described. The upper housing portion 67 and the items connected to it can be reciprocated together horizontally relative to the central housing portion 68 by a rack and pinion drive or other suitable drive mechanism. In Figure 11, the rack and pinion drive is hidden from the figure and represented by a dashed line, and is identified overall by reference number 70.

[0062] Figure 11 also shows the housing 71 for the magnetron 15 (Figure 1). The magnetron 15 generates microwave energy that is supplied to the microwave cavity 72. The microwave cavity 72 can be a single-mode cavity that is waveguide-connected to the magnetron 15.

[0063] Figure 12 is a cross-sectional view taken substantially along line 12-12 in Figure 11. Figure 12 shows the upper housing portion 67 and the central housing portion 68, as well as some of the components therein. In the orientation of Figure 12, the master displacement member 36 (e.g., a piston) and the master chamber 38 (e.g., a cylinder or annular sleeve) are shown at least partially as cross-sections taken perpendicular to their longitudinal axes. The master chamber 38 can be a cylindrical passage horizontally opened within the upper body 74 of the instrument 66. In the illustrated embodiment, the master displacement member 36 and at least one wall of the master chamber 38 define an elongated annular space coaxial with the master displacement member and containing part of the hydraulic fluid. The hydraulic fluid is shown only in Figure 1 and is schematically represented by pointillism.

[0064] The slave chamber 42 can be a cylindrical passage opened perpendicularly to the upper body 74. The slave displacement member 40 (e.g., a piston) may have a somewhat H-shaped cross-section, the upper part of which defines a cavity 75 into which the hydraulic fluid extends. In some implementations, the upward-opening cavity 75 at the upper end of the slave displacement member 40 may be omitted. The hydraulic slave chamber 42 (e.g., a cylinder or annular sleeve) is hydraulically connected to the hydraulic master chamber 38 via a hydraulic passage 31 (Figure 1) of the hydraulic circuit, as will be further described below. The hydraulic circuit 20 (Figure 1) can be filled with hydraulic fluid through a filling hole 76 which is closed by a plug 78 in Figure 12.

[0065] The slave displacement member 40 can be mounted movably to reciprocate within the upper body 74 by at least one or assembly of mounting and / or sealing components 80. The extension member 82 can be fixedly mounted to the lower end of the slave displacement member 40 (for example, by a threaded shaft extending into a threaded bore) so that the extension member and the slave displacement member reciprocate together. The slave displacement member 40 and the extension member 82 may together be referred to as plungers 40 and 82, which are mounted to reciprocate upright within the internal space of a downward-opening body or assembly, including the upper body 74, the lower body 84, and a plate 86 with through holes. If necessary, the slave displacement member 40 and the extension member 82 can be formed as a single part. However, in practice, using separate parts makes it easier to form the slave displacement member 40 with relatively close tolerances and therefore potentially less expensive, while the extension member 82 can be formed with wider tolerances. Like many other parts of the apparatus 66, the displacement members 36, 40, the main body parts 74, 84, and the plate 86 can be made of a metallic material.

[0066] The upper body 74, lower body 84, and plate 86 together may be called the inner housing or body 74, 84, 86, which is carried by the upper housing portion 67 when the upper housing portion reciprocates horizontally relative to the central housing portion 68. The inner body 74, 84, 86 may be formed from fewer or more parts. In Figure 12, the plungers 40, 82 are in an upper position or a retracted position within the internal space of the downward-opening inner body 74, 84, 86.

[0067] The slave displacement member 40, more specifically the plungers 40, 82, can be biased toward a retracted position by at least one helical compression spring 88 extending around the extension member 82. The spring 88 may have ends that engage with a lower annular flange protruding outward from the slave displacement member 40 and a lower annular flange protruding inward from the mounting sleeve 90, respectively. The upper annular flange protruding outward from the mounting sleeve 90 can be fixedly attached to the upper body 74 by fasteners and / or any other suitable device. The upper surface of the outwardly extending annular lower flange of the extension member 82 can engage with the lower surface of the lower flange of the mounting sleeve 90 to restrict or prevent the upward movement of the plungers 40, 82.

[0068] Continuing to refer to Figure 12, the support or holder of the container 12 may include an upward-opening receptacle 92 fixedly mounted to the central housing portion 68 to removably receive and securely support the container 12. The support in the form of the receptacle 92 may include at least one side wall 94 extending around the upward-opening internal space of the receptacle. The lower inner surface of the receptacle side wall 94 may be cylindrical and have a lateral dimension or diameter slightly larger than the outer lateral dimension or diameter of the cylindrical portion of the container 12. The annular inner surface of the upper portion of the receptacle side wall 94 may taper in a direction along the height of the receptacle 92 to define a frustoconical inner surface 96 of the receptacle. The frustoconical inner surface 96 may define an upper opening to the receptacle 92. The lateral dimension or diameter of the frustoconical inner surface 96 increases vertically along the height of the receptacle 92. The frustum surfaces 50 and 96 have the same or nearly the same inclination and are in face-to-face contact with each other, distributing the forces based on contact between them over a wide surface area, thereby reducing the force (stress) per unit area, compared to typical flange base engagements.

[0069] In Figure 12, as described above with reference to Figures 9 and 10, the cap assembly 14 is attached to the upper end of the container 12, and the lower ends of the plungers 40, 82 are positioned above the cap assembly and spaced apart from it. Repeating from above, in Figure 12, the plungers 40, 82 are in their upper or retracted position. In the illustrated embodiment, the plungers 40, 82, or more specifically the extension member 82, are fitted with several mechanisms for engaging and / or cooperatively associating with the cap assembly 14 on the container 12, which is supported by the holder or receptacle 92. Alternatively, in some embodiments, the slave displacement member 40 or the extension member 82 may be configured to be more directly associated with the cap assembly 14 (e.g., directly engaged).

[0070] In the example shown in Figure 12, the engager 100 (e.g., engagement device) reciprocates with the plungers 40, 82 and is fixedly connected to the extension member 82 to engage with the cap assembly 14. The engager 100 can be formed from a single part or multiple parts. In the example shown in the drawings, the inner portion of the engager or engagement device 100 includes a backing structure in the form of an annular backplate 102. The inner portion of the engagement device may further include an annular sleeve 104 extending upward from the periphery of the backplate 102 and an annular flange 106 extending downward from the annular sleeve 104 and / or the backplate 102. The backplate 102 can be fixedly connected to the flange of the extension member 82, for example, using appropriate mechanical fasteners. The lower surface of the backplate 102 may have a wavy shape, as will be further described below. As with many other parts of the fixture 66, the extension 82 and the inner portion of the engagement device 100 can be formed from a metallic material.

[0071] The inner portion of the engagement device 100 can be fixedly and securely connected to the outer portion of the engagement device. The outer portion of the engagement device 100 may include an engagement disc 110, an annular U-shaped channel 112, and an annular sleeve 114. The annular inner wall of the channel 112 may extend downward from the periphery of the engagement disc 110. The sleeve 114 may extend upward from the annular outer wall of the channel 112 and be engaged by sliding contact with a coaxial cylindrical inner surface (e.g., guide channel) of the lower body 64 on a facing surface. The flange 106 of the inner portion of the engagement device 100 can be fitted (e.g., interlocked) into the annular opening defined by the channel 112. The outer portion of the engagement device 100 may be made of an elastic (e.g., flexible) material, such as a polymer material. As an example, the outer portion of the engagement device 100 may be made of a thermosetting polymer material such as synthetic rubber (e.g., neoprene or polychloroprene), but is not limited to this. As a more specific example, the outer portion of the engagement device 100 can be made of a thermoplastic polymer material such as a fluorocarbon solid (e.g., a perfluoroalkoxyalkane), but is not limited to this. The outer portion and / or multiple portions of the engagement device 100 can take the form of a film or flexible film, and / or be referred to as a film or flexible film. Thus, the disk 110 can be referred to as a flexible engagement web or flexible engagement film, and may have a wavy shape, as will be further described below.

[0072] Continuing to refer to Figure 12, the force sensor 26 is positioned within the internal cavity of the extension member 82, as will be further described below, and can be operably associated via a link with the central portion of the disk 110 (e.g., the engagement membrane). In Figure 12, the plungers 40, 82 are in the upper configuration, along with the engagement device 100, in response to a spring 88 that is extended in response to relatively low hydraulic pressure in the hydraulic system. In contrast, in Figures 13-15, in response to relatively high hydraulic pressure in the hydraulic system, the plungers 40, 82 are in the lower configuration, along with the engagement device 100, and the spring 88 is compressed.

[0073] Referring to Figures 14 and 15, the actuator 16 may take the form of an electric motor that rotationally drives a motor gear 120. Referring to Figure 16, the motor gear 120 can reciprocate by meshing with a lead gear 122. The lead gear 122 is coaxial with the shaft of the lead screw 124 and can be fixedly mounted to the shaft in order to rotate the lead screw 124. The male(s) thread(s) of the lead screw 124 can mesh with the female(s) thread(s) of a drive nut 126 that is supported to reciprocate along a guide path. A master displacement member 36 may be connected to or otherwise associated with the drive nut 126 to reciprocate with the drive nut in response to the operation of the actuator or motor 16. One or more spring washers may be positioned within the cavity of the drive nut 126 and engaged with the outer end of the master displacement member 36. Alternatively, the drive nut 126 may be replaced with a ball screw or other suitable device for converting rotational motion into linear motion.

[0074] The master displacement member 36 can be mounted to move reciprocatingly within the upper body 74 by at least one of the mounting parts 130 and / or sealing parts 130 or an assembly thereof. The hydraulic circuit 20 (Figure 1) may include at least one other hole 132 configured for use in filling and / or venting the hydraulic circuit, the hole 132 is typically closed by a plug (see, for example, plug 78).

[0075] Referring to Figure 17, the master chamber 38 and slave chamber 42 can be elongated holes in the upper body 74, and the axes of these chambers can extend laterally (e.g., perpendicularly) to each other. Similarly, the hydraulic passage 31 connecting the chambers 38 and 42 can be an elongated hole in the upper body 74. The pressure sensor 24 can be mounted on the outer end of the hydraulic passage 31.

[0076] Figure 18 is a cross-sectional view showing plungers 40, 82 and engaging device 100 in the lower configuration, such that the lid 58 is clamped downwards to close the container 12 while the pressure inside the container is equal to the ambient pressure (for example, so that the lid does not expand upwards).

[0077] In the example shown in Figure 18, the engaging membrane or disk 110 includes an annular, downwardly projecting central portion (e.g., an inner projection 140) and an annular, downwardly projecting outer portion (e.g., an outer projection 142) extending around and spaced apart from the central portion. As a result, the engaging disk 110 (e.g., membrane) defines an upwardly extending, annular, recessed cavity 144 located between the inner projection 140 and the outer projection 142.

[0078] The backplate 102 may include a through hole 150 and a portion (e.g., projection 152) that extends substantially around the hole 150 and projects downward at a distance from the hole 150. The outer projection 142 of the engaging disc may be defined by an annular ridge in the engaging film or the web material of the disc 110, the upper side of which may define an annular channel from which the backplate projection 152 extends. The backplate projection 152 may define a downwardly open annular channel from which the engaging ring 154 is received (e.g., press-fitted). The engaging ring 154 may be made of a softer and more elastic material than the backplate 102. For example, the engaging ring 154 may be an O-ring made of a flexible elastomer polymer configured to provide compliance and improve sealing efficiency (e.g., the lower part of the engaging ring 154 may project downward outward from the backplate 102 or the backplate projection 152).

[0079] The extension member 82 may include a lower annular flange 156 extending through the backplate hole 132. The extension flange 156 may define an opening to the cylindrical cavity 158. The force sensor 26 is positioned within the extension cavity 158 and can directly or indirectly engage with the inside of the inner projection 140 of the engaging disk. In Figure 18, the linkage positioned within the extension cavity 158 between the force sensor 26 and the inner projection 140 includes a series arrangement of a disk 160 and one or more sleeves 162, 164. The disk 160 and sleeves 162, 164 are slidable and reciprocating within the extension cavity 158 to transmit force to the force sensor 26.

[0080] As shown in Figure 19, in an example where the container 12 is sealed and contains contents under pressure, the upward force exerted by the bent (e.g., inflated) lid 58, indicating the pressure inside the container 12 (circularly shown by the upright arrow in Figure 19), is transmitted to the force sensor 26 via the disk 160 and sleeves 162, 164. Alternatively, the force in question can be received by the force sensor 26 in a relatively more or less direct manner.

[0081] In the example shown in Figure 19, a portion of the bent (e.g., expanded) lid 58 partially extends into a recessed cavity 144 of the engagement disc or membrane 110. Generally speaking, the recessed cavity 144 is a geometric feature that helps produce more accurate measurements of the pressure inside the container 12 by accommodating, for example, a portion of the lid 58 (e.g., displaced material). The clamping process may, for example, crush a portion of the lid 58 adjacent to a clamping projection 142, causing the displaced portion of the lid to move into the cavity 144 in an attempt to avoid inaccurate measurements by the force sensor 26. In another example, the lid 58 may expand when heated, and the recessed cavity may adapt to such expansion in an attempt to avoid inaccurate measurements by the force sensor 26. The geometric features, more specifically the cavity 144, may be configured differently.

[0082] In the example shown in Figure 20, the container 12 is slightly open to accommodate contents under pressure, but the pressure is reduced by ventilation from the container to the outside through at least one gap defined between the underside of the lid 58 and the mouth of the container 12 (e.g., the seat 56 (Figure 2)). In Figure 20, the size of the gap is exaggerated for illustrative purposes. One or more ventilation passages schematically represented by the lower arrows in Figure 20 may extend through one or more band slots 65 (Figures 5-10) or other suitable openings or gaps.

[0083] In Figure 20, during ventilation, the container 12 remains partially closed by the lid 58 (for example, the lid completely blocks the container opening 48), so an upward force is continuously applied to the lid 58, and a force indicating the pressure inside the container 12 is transmitted to the force sensor 26 via the disc 160 and sleeves 162, 164.

[0084] Figure 21 is an exploded view of the many components of the device 66 (Figures 11-15). For example, some of the mechanical fasteners that connect the components to each other are indicated by reference numeral 170 in Figure 21.

[0085] Figure 22 is a chart showing the operating parameters of an exemplary pressure-stepped decomposition chemical reaction performed using apparatus 66, including periodic ventilation from the headspace of the associated vessel 12. In Figure 22, the chart's key or legend identifies lines representing the temperature of the contents in vessel 12, the pressure inside the vessel, and the pressure of the fluid in the hydraulic circuit 20, respectively. The left vertical axis contains a scale for the temperature of the contents in vessel 12. The right vertical axis contains a scale for the pressure of the fluid in the hydraulic circuit 20. A relatively thin line representing the pressure inside vessel 12 is superimposed on the graph shown in Figure 22 to show the relationship between the pressure inside the vessel and the hydraulic pressure in the hydraulic circuit 20.

[0086] Various examples are described below with reference to the example shown in Figure 22. In Figure 22, each of the seven periods of ventilation from the container 12 can be identified by a portion of the line representing the pressure inside the container, which slopes "substantially" downward to the right from the peak to the lowest point, and coincides perpendicularly with both (i) the portion of the line representing the hydraulic pressure that slopes "substantially" downward to the right from the peak to the lowest point, and (ii) the portion of the line representing the temperature inside the container that slopes "substantially" downward to the right from the peak to the lowest point. There may be fewer than seven ventilation periods or more than seven ventilation periods (for example, there may be one or more ventilation periods from the container 12).

[0087] Each of the line segments described above as "sloping 'substantially' downward from the peak towards a lower point" can be referred to as a backslash segment (e.g., "\") for ease of reference. In contrast, line segments sloping upward from a lower point towards the peak can be referred to as a slash segment (e.g., " / ") for ease of reference. In Figure 22, at least some of the peaks of the lines representing the internal pressure or each backslash segment (e.g., "\") can be referred to as the internal pressure vent points. In Figure 22, at least some of the peaks of the slash segments (e.g., " / ") representing the hydraulic pressure can be referred to as hydraulic pressure setpoints, and / or at least some of the nearly horizontal segments of the lines representing hydraulic pressure that precede the backslash segments (e.g., "\") can be referred to as hydraulic pressure setpoints.

[0088] Figure 23 shows a flowchart of an example of a method (circularly represented by blocks 500-530 in Figure 23) relating to an exemplary pressure-stepped decomposition chemical reaction, for example, represented by the chart in Figure 22, in relation to the system schematically depicted in Figure 1. Referring mainly to Figure 23 and occasionally to Figure 1, in block 500, the controller or processor of computer 30 may provide and receive signals to the computer's graphical user interface to facilitate the user selecting a pre-programmed method of operating the apparatus 66 (Figures 11-15) or to generate a custom method of operation. For example, in block 500, the processor may, in response to user input, facilitate the programming of at least the following parameters: sample temperature - set the desired sample peak temperature in the vessel 12; ramp time - set the time from the ambient temperature in the vessel to the desired sample peak temperature in the vessel; holding time - set the amount of time to hold the desired sample peak temperature in the vessel; control pressure - set the maximum desired pressure in the vessel; vent points - set the desired number of pressure vent points in the vessel (e.g., the number of vent cycles).

[0089] Processing control is transferred from block 500 to block 505. Blocks 505 to 530 can generally represent do-loops or for-loops that are performed or executed in a sequential manner in relation to each venting period from the container 12. For example, blocks 505 to 530 may be executed in the first venting period, then blocks 505 to 530 may be executed in the second venting period, and so on.

[0090] In block 505, the hydraulic setpoint is calculated by the processor relative to the corresponding vessel pressure vent point. Repeating from above, in Figure 22, the peak of the slash portion (e.g., " / ") of the line representing hydraulic pressure can be called the hydraulic setpoint, and the peak of the backslash portion (e.g., "\") of the line representing vessel pressure can be called the vessel pressure vent point. The hydraulic setpoint can be based on the parameters of gradient, offset, and cushion. The gradient parameter can be from an empirically determined curve of the hydraulic pressure required to maintain a given vessel pressure using the clamping device, vessel 12, and cap assembly 14 (e.g., band 57 and lid 58 (e.g., bulkhead)). The offset parameter may be a value used to account for any sealing inefficiencies between the vessel 12 and lid 58, which are due to, but not limited to, physical parameters such as surface finish and tolerances. The cushion parameter may be an offset that can be added as an additional safety factor in an attempt to ensure a robust seal between the lid 58 and the vessel 12. Processing control is transferred from block 505 to block 510.

[0091] In block 510, the processor causes the fluid pressure in the hydraulic circuit 20 to reach a hydraulic setpoint. In this iteration, the hydraulic setpoint is sufficiently high to restrict any early venting from the vessel 12. In response to one or more signals in block 510, the motor 16 operates (for example, in the forward rotation direction), and the master displacement member 36 moves responsively until it reaches the hydraulic setpoint, as indicated by the hydraulic sensor 24. The operation of the motor 16 is stopped in response to an indication that the hydraulic setpoint has been reached. In response to the resulting pressure in the hydraulic circuit 20, the vessel 12 is sealed closed by the lid 58, for example, as described above. Processing control then moves from block 510 to block 515.

[0092] In block 515, the processor transmits a signal(s) such as, for example, by using microwaves from the microwave source 15 to heat the contents of container 12, as described above. In response to the heating, the temperature and pressure inside container 12 increase. More specifically, the microwaves increase the temperature of the sample inside container 12, and the increase in pressure inside the container is a byproduct of the increase in the sample's temperature.

[0093] Simultaneously with block 515, in block 520, the processor receives signals indicating the pressure and / or temperature inside the container 12. For example, the processor may receive signals from both the temperature sensor 28 and the force sensor 26. Again, the signal from the temperature sensor indicates the temperature inside the container 12, and the signal from the force sensor 26 indicates the pressure inside the container 12. In block 520, a decision is made as to whether outward ventilation from the container 12 is initiated. For example, microwaves (see, for example, block 515) may be continuously applied to the contents of the container 12 to increase the temperature of the sample inside the container 12 until (i) a temperature setpoint is reached (the system may then maintain the sample temperature for a set holding time), or (ii) the container pressure reaches a desired ventilation pressure (e.g., container pressure ventilation point). Based on the signal from the temperature sensor 28, the processor may determine whether the temperature setpoint has been reached. Based on the signal from the force sensor 26, the processor may determine whether the container pressure ventilation point (e.g., the setpoint) has been reached. Referring to Figure 22 and repeating from above, the peak of the backslash portion (e.g., "\") of the line indicating the internal pressure of the vessel can be called the internal pressure vent point. In response to the positive decision in block 520, processing control is transferred to block 525.

[0094] In block 525, a signal from the processor and / or a cessation of the signal causes the microwave source 15 to stop operating in order to cease heating the contents of the container, and ventilation from the container 12 is initiated. In response to one or more signals in block 525, the motor 16 operates in the reverse direction and the master displacement member 36 moves responsively to reduce the pressure in the hydraulic circuit 20 in order to initiate and control the ventilation from the container 12. In response to feedback signals received by the processor and signals from the processor to the motor 16, the pressure in the hydraulic circuit 20 is reduced so that the pressure in the container 12 decreases at an appropriate gradient (e.g., speed) and restricts ventilation in the manner described above (e.g., to ensure that only gas from the headspace of the container is vented (e.g., typically without venting any analytes from the container)). For example, the system can reduce the pressure inside the container based on pressure delta and pressure gradient parameters. The pressure delta parameter determines or defines the total pressure drop inside the container. The pressure gradient parameter determines or defines the speed at which the system achieves the pressure drop inside the container. For example, the motor 16 can be operated in reverse to reduce the clamping force on the lid 58 at a motor speed determined or defined by the pressure gradient parameter, while the internal pressure of the container is monitored by the force sensor 26 and fed back to the processor for control operations (e.g., adjusting the motor speed), and is utilized by the processor.

[0095] Simultaneously with block 525, in block 530, the processor may determine, based on the signal from the force sensor 26, whether a predetermined decrease in the internal pressure of the vessel has occurred (for example, whether the bottom of each backslash portion (e.g., "\") of the line indicating the internal pressure of the vessel has been reached, referring to Figure 22). Once the processor determines, based on the signal from the force sensor 26, that a desired internal pressure difference has been met (e.g., determined or defined by the pressure delta parameter), processing control is transferred to block 505 to initiate the next iteration through blocks 505-530. However, the sequence through blocks 505-530 can be arranged differently. For example, the calculation in block 505 may be performed for each iteration (e.g., vent point) before proceeding to block 510, resulting in the processor generally looping through blocks 510-530 several times after block 505. Other modifications are also within the scope of this disclosure.

[0096] To repeat at least partially the above, in one aspect of the present disclosure, the pressure and closing force inside the container 12 are both measured at least indirectly, and during the venting process, the closing force can be adjusted to substantially match (e.g., slightly less than) the pressure of the contents inside the container. The closing force can be matched, for example, to within about 50 pounds per square inch of the pressure inside the container 12, and in some cases to within about 10 pounds per square inch or less of the pressure inside the container.

[0097] Partially opening the vessel 12 for ventilation purposes while the pressures are substantially matched helps to avoid any kind of spray, aerosol, or complete liquid ejection that might otherwise occur. Thus, in exemplary manner, the reaction vessel 12 is opened for ventilation while the respective pressures are matched to within approximately 50 pounds / square inch, matched to within approximately 10 pounds / square inch, or matched to less than 10 pounds / square inch.

[0098] Since the reactions being tested are often decomposition reactions, the temperature inside container 12 is typically higher than the boiling point of water, sometimes maintained at around 300–350°C. Similarly, the pressure inside container 12 is typically at least about 250 pounds per square inch, often exceeding 500 pounds per square inch, and sometimes reaching about 700–750 pounds per square inch. In some implementations, the pressure inside the container is not permitted to exceed 750 pounds per square inch.

[0099] Repeating at least partially the above, the system 10, and therefore the apparatus 66, typically includes at least one controller 30 operably associated with a number of electrical components of the system (e.g., microwave sources, sensors, motors, and / or other suitable components). The at least one controller 30 may include one or more computers, computer data storage devices, programmable logic devices (PLDs), and / or application-specific integrated circuits (ASICs). A suitable computer may include one or more of the following: a central processing unit (CPU) or processor, an integrated circuit or memory, a user interface (e.g., a graphical user interface), peripheral or device interfaces for interfacing with other electrical components of the system, and / or other arbitrary suitable features. Each controller(s) may communicate with the electrical components of the system by a suitable signaling path. The processes of the present disclosure may be controlled (e.g., at least partially controlled) in response to the execution of a computer-based algorithm operably associated with at least one controller 30. Controller 30 is schematically represented as a rectangle identified by the number 30 in Figure 1, and other components or features mentioned in this paragraph are schematically represented by rectangles located within the rectangle identified by the number 30 in Figure 1.

[0100] Repeating the above at least partially, various different configurations of clamping devices are included within the scope of this disclosure. For example, in an alternative embodiment, the hydraulic circuit 20 (Figure 1), and optionally the spring 88 (Figure 12), can be eliminated, the orientation of the upstream linkage 18 (Figure 1) can be changed so that the lead screw 124 (Figure 16) rotates around the upright axis and the drive nut 126 (Figure 16) reciprocates along the upright axis, and an extension member 82 (Figure 12) can be fixedly attached to the lower end of the drive nut 126 so that the extension member and the drive nut reciprocate together. In such an alternative embodiment, the pressure sensor 24 (Figure 1) can be replaced with a suitably mounted force sensor configured to measure the closing force provided by the alternative clamping device. Such a force sensor may be a load cell arranged in series with each component of the alternative clamping device. Thus, in this alternative embodiment, throughout the foregoing, hydraulic adjustments can be replaced with other suitable (e.g., purely mechanical) adjustments.

[0101] To supplement this disclosure, this application fully incorporates, by reference, the following U.S. patents: No. 9,237,608; No. 9,943,823; and No. 10,527,530.

[0102] To reiterate, for the purpose of providing a broad disclosure, it is within the scope of this disclosure that one or more terms such as “substantially,” “about,” and “approximately” modify each of the adjectives and adverbs of the foregoing disclosure. For example, it is considered that a person skilled in the art will readily understand that reasonably different engineering tolerances, accuracy, and / or precision may be applicable and appropriate to obtain the desired results in different implementations of the features of this disclosure. Accordingly, it is considered that a person skilled in the art will readily understand the use of terms such as “substantially,” “about,” and “approximately” as used herein.

[0103] Examples of embodiments are disclosed in this specification and in the drawings. The present invention is not limited to such exemplary embodiments. The use of the term "and / or" includes any and all combinations of one or more of the related enumerated items. Unless otherwise noted, specific terms are used in a general and descriptive sense and are not intended to be limiting.

Claims

1. A system for carrying out a decomposition reaction, the system is A support configured to support the reaction vessel, A clamping device configured to apply a closing force toward the mouth of the reaction vessel while the reaction vessel is supported by the support, A heating device configured to heat the contents of the reaction vessel while the reaction vessel is supported by the support, A first sensor configured to provide a signal indicating the gas pressure in the headspace of the reaction vessel while the reaction vessel is supported by the support, A second sensor configured to provide a signal indicating the closing force, A computer configured to control the closing force and the ventilation outward from the opening of the reaction vessel via a clamping device in response to an input while the reaction vessel is supported by the support, wherein the input includes the signal from the first sensor and the signal from the second sensor, and A system equipped with these features.

2. The clamping device includes an engaging portion configured to reciprocate toward and away from the support, and the system is The reaction vessel, An elastic partition wall is configured to be clamped between the mouth of the reaction vessel and the engaging portion. The system according to claim 1, comprising:

3. It is equipped with a band, and the band is A body that extends at least partially around the hole and defines the hole, A plurality of latches extending downward from the main body, wherein the plurality of latches are configured to removably attach the band and the partition to the opening of the reaction vessel by elastically deforming and removably engaging with a predetermined portion of the reaction vessel, and The system according to claim 2, comprising:

4. The clamping device comprises a hydraulic system and a motor configured to operate in such a way as to increase the hydraulic pressure within the hydraulic system. The system according to claim 1, wherein the clamping device is configured to increase the closing force in response to an increase in hydraulic pressure within the hydraulic system.

5. The support comprises a receptacle, The receptacle has a frustoconical inner surface configured to face and make direct contact with the reaction vessel, The frustoconical inner surface has a variable diameter, The system according to claim 1, wherein the diameter of the frustoconical inner surface increases in the vertical direction.

6. The clamping device comprises a hydraulic system having a displacement member that is at least partially positioned within the chamber, The chamber and the displacement member are configured cooperatively such that the displacement member moves outward relative to the chamber in response to an increase in hydraulic pressure within the hydraulic system. The clamping device is configured to apply the closing force in response to the displacement member moving outward relative to the chamber. The system according to claim 1, wherein the second sensor is a hydraulic sensor configured to provide a signal indicating hydraulic pressure in the hydraulic system.

7. The system according to claim 6, wherein the hydraulic sensor is installed in an opening into the hydraulic passage of the hydraulic system.

8. The chamber of the hydraulic system is a cylinder, The hydraulic system according to claim 7, wherein the displacement member of the hydraulic system is a piston that is at least partially positioned within the cylinder.

9. The system according to claim 6, comprising at least one spring, wherein the system is configured such that, in response to a decrease in hydraulic pressure in the hydraulic system, a force from the at least one spring biases the displacement member to move inward relative to the chamber.

10. The clamping device comprises an enforcer connected to the displacement member for movement together with the displacement member, The clamping device is configured to clamp a portion of the closure between the lower part of the annular portion of the engager and the opening of the reaction vessel while the reaction vessel is supported by the support, The annular portion of the engager extends around the central portion of the engager, The system according to claim 6, wherein the first sensor is cooperatively associated with the central portion of the engager to provide the signal indicating the gas pressure in the headspace of the reaction vessel while the reaction vessel is supported by the support.

11. comprising a main body, The chamber of the hydraulic system is provided with a hole defined in the main body, The system according to claim 6, wherein the displacement member is mounted to reciprocate in the hole in response to a predetermined fluctuation in the hydraulic pressure within the hydraulic system.

12. The hole is a first hole, The hydraulic system is provided with a second hole defined in the main body, The system according to claim 11, wherein the second hole is in fluid communication with the first hole.

13. The system according to claim 12, wherein the hydraulic system comprises a displacement member mounted to reciprocate in the second hole in response to the operation of a motor.

14. The first hole is elongated and defines a longitudinal axis, The second hole is elongated and defines a longitudinal axis, The system according to claim 13, wherein the longitudinal axis of the first hole extends laterally with respect to the longitudinal axis of the second hole.

15. The system comprises a sleeve that is fixedly attached to the main body, The sleeve is equipped with a flange that extends inward, The system according to claim 11, further comprising at least one spring positioned between the flange and the displacement member, wherein a force from the at least one spring biases the displacement member in response to a decrease in hydraulic pressure in the hydraulic system, causing it to move inward relative to the chamber.

16. The end of at least one spring is engaged with the flange, The system according to claim 15, wherein the end of at least one spring is engaged with the displacement member.

17. A system that performs a decomposition reaction, the system is A support configured to support the reaction vessel, A clamping device equipped with an engagementr, The clamping device is configured to clamp at least a portion of the closure between the underside of the engager and the mouth of the reaction vessel while the reaction vessel is supported by the support, The lower side of the engager has an upward-extending recess that extends at least partially around the downward-extending portion of the engager, a clamping device, A force sensor, wherein the force sensor is cooperatively associated with the downward projection of the closure, to provide a signal indicating the pressure inside the reaction vessel while at least a portion of the closure is clamped between the lower side of the closure and the opening of the reaction vessel. It is equipped with, The system is configured such that the upward-extending recess is adapted to the upward movement of a portion of the closure in order to improve the accuracy of the signal from the force sensor.

18. The system according to claim 17, wherein the upwardly extending recess is configured to partially adapt to the upward expansion of the closure in order to improve the accuracy of the signal from the force sensor.

19. The engager is a flexible engaging web which is part of the engaging device. The engagement device further comprises a backing structure configured to press the engagement web toward the mouth of the reaction vessel while the reaction vessel is supported by the support, The system according to claim 17, wherein the backing structure is more rigid than the engaging web, defines a through-hole, and through the through-hole, the force sensor is cooperatively associated with the downward projection of the engaging web so as to provide the signal indicating the pressure inside the reaction vessel while the portion of the closure is clamped between the underside of the engaging web and the mouth of the reaction vessel.

20. The clamping device comprises a hydraulic system and a motor configured to operate in such a way as to increase the hydraulic pressure within the hydraulic system. The system according to claim 17, wherein the clamping device is configured to increase the closing force in response to an increase in hydraulic pressure in the hydraulic system.

21. The support comprises a receptacle, The receptacle has a frustoconical inner surface configured to face and make direct contact with the reaction vessel, The frustoconical inner surface has a variable diameter, The system according to claim 17, wherein the diameter of the frustoconical inner surface increases in the vertical direction.

22. The clamping device is configured to apply a closing force toward the opening of the reaction vessel while the reaction vessel is supported by the support, The system according to claim 17, further comprising a second sensor configured to provide a signal indicating the closing force.

23. The clamping device comprises a flexible engaging member, The clamping device is configured to clamp at least a portion of the closure between the lower side of the flexible engaging member and the opening of the reaction vessel while the reaction vessel is supported by the support, The flexible engaging member comprises both a downwardly projecting central portion and a downwardly projecting outer portion that extends at least partially around the downwardly projecting central portion. The lower side of the flexible engaging member defines an upwardly extending recessed cavity, The upward-extending recessed cavity extends at least partially around the downward-projecting central portion of the flexible engaging member, The upward-extending recessed cavity is positioned between the downward-extending central portion of the flexible engaging member and the downward-extending outer portion of the flexible engaging member, such that the downward-extending outer portion of the flexible engaging member extends at least partially around the upward-extending recessed cavity defined by the lower side of the flexible engaging member. The force sensor is associated cooperatively with the downwardly projecting central portion of the flexible engaging member to provide the signal indicating the pressure inside the reaction vessel while at least a portion of the closure is clamped between the lower side of the flexible engaging member and the opening of the reaction vessel, and the system is configured to transmit force to the force sensor at least through the central portion of the flexible engaging member. The system according to claim 17, wherein the upward-extending recessed cavity defined by the flexible engaging member is configured to adapt to the upward movement of the portion of the closure in order to improve the accuracy of the signal from the force sensor.

24. The system according to claim 23, wherein the upward-extending recessed cavity is configured to include an upward-extending recessed cavity that is open downward and empty, so that when the system is in operation, the outward-bending portion of the closure can extend upward to the upward-extending recessed cavity.

25. The intermediate portion of the flexible engaging member is positioned between the downwardly protruding central portion of the flexible engaging member and the downwardly protruding outer portion of the flexible engaging member, The system according to claim 23, wherein the downwardly projecting central portion of the flexible engaging member extends downward from the intermediate portion of the flexible engaging member such that the lower surface of the intermediate portion of the flexible engaging member at least partially defines the upwardly extending recessed cavity, and the upper surface of the downwardly projecting central portion of the flexible engaging member at least partially defines the downwardly extending recessed cavity.

26. The system according to claim 23, further comprising a linkage positioned between the force sensor and the upper surface of the downwardly protruding central portion of the flexible engaging member and engaging with the force sensor and the upper surface of the downwardly protruding central portion of the flexible engaging member, wherein the linkage is configured to transmit force from the downwardly protruding central portion of the flexible engaging member to the force sensor.

27. ​​The intermediate portion of the flexible engaging member is positioned between the downwardly protruding central portion of the flexible engaging member and the downwardly protruding outer portion of the flexible engaging member, The system according to claim 26, wherein the downwardly projecting central portion of the flexible engaging member extends downward from the intermediate portion of the flexible engaging member such that the lower surface of the intermediate portion of the flexible engaging member at least partially defines the upwardly extending recessed cavity, and the upper surface of the downwardly projecting central portion of the flexible engaging member at least partially defines the downwardly extending recessed cavity, and the lower end of the linkage extends to the downwardly extending recessed cavity.

28. The flexible engaging member is an engaging disc of an engaging device, The engagement device further comprises an annular channel and an annular sleeve, The inner annular wall of the channel extends downward from the periphery of the engaging disk. The system according to claim 23, wherein the sleeve extends upward from the outer annular wall of the channel.

29. The system according to claim 23, wherein the flexible engaging member is a flexible film.

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