SAMPLING ARRANGEMENT

Abstract

The invention provides a sampling arrangement (105) for sampling from a reactor (50), the sampling arrangement (105) comprising a gas inlet (110), a solvent inlet (120), a solvent compartment (130), one or more multiple-position valves (140), a sampling compartment (150), and an outlet, wherein in a first operational mode (10) the one or more multiple-position valves (140) are configured to provide: fluid contact between the solvent inlet (120) and the solvent compartment (130); fluid contact between the reactor (50) and the sampling compartment (150); and fluid separation between the solvent compartment (130) and the sampling compartment (150); and wherein in a second operational mode (20) the one or more multiple-position valves (140) are configured to provide: fluid contact between the gas inlet (110), the solvent compartment (130), the sampling compartment (150), and the outlet (160).

Claims

1. A sampling arrangement (105) for sampling from a reactor (50), the sampling arrangement (105) comprising a gas inlet (110), a solvent inlet (120), a solvent compartment (130), one or more multiple-position valves (140), a sampling compartment (150), and an outlet, wherein in a first operational mode (10) the one or more multiple-position valves (140) are configured to provide: fluid contact between the solvent inlet (120) and the solvent compartment (130); fluid contact between the reactor (50) and the sampling compartment (150); and fluid separation between the solvent compartment (130) and the sampling compartment (150); and wherein in a second operational mode (20) the one or more multiple-position valves (140) are configured to provide: fluid contact between the gas inlet (110), the solvent compartment (130), the sampling compartment (150), and the outlet (160).

2. The sampling arrangement (105) according to claim 1, wherein the one or more multiple-position valves (140) comprises a 10-position valve, wherein the 10-position valve is configurable in a first configuration and in a second configuration, wherein the sampling arrangement (105) is in the first operational mode (10) when the 10-position valve is in the first configuration, and wherein the sampling arrangement (105) is in the second operational mode (20) when the 10-position valve is in the second configuration.

3. The sampling arrangement (105) according to claim 1, wherein the sampling compartment (150) has a sampling volume V.sub.150 selected from a range of 50 μl-5 ml, and wherein the solvent compartment (130) has a solvent volume V.sub.130, wherein V.sub.130≥2*V.sub.150.

4. The sampling arrangement (105) according to claim 1, wherein during operation of the sampling arrangement (105) the sampling compartment (150) is arranged external to the reactor (50).

5. A system (100) comprising the sampling arrangement (105) according to claim 1, wherein the system (100) comprises a control system (300), wherein the control system (300) is configured to control the one or more multiple-position valves (140), and wherein the control system (300) is configured to in a first mode of operation consecutively execute the first operational mode (10) and the second operational mode (20).

6. The system (100) according to claim 5, wherein the system (100) comprises or is functionally coupled to a solvent supply (125), wherein the solvent supply (125) is fluidically coupled to the solvent inlet (120), wherein the system (100) comprises a solvent supply pressurizer (121) configured to pressurize the solvent supply (125) during the first operational mode (10).

7. The system (100) according to claim 5, wherein the system (100) comprises or is functionally coupled to a dispenser valve (164), wherein the outlet (160) is functionally coupled to the dispenser valve (164), and wherein the dispenser valve (164) is configured to dispense fluid to one or more outlet containers (60).

8. The system (100) according to claim 5, wherein the system (100) further comprises a pump (170), wherein in the first operational mode (10) the one or more multiple-position valves (140) are configured to provide a fluid contact between the pump (170), the sampling compartment (150) and the reactor (50).

9. The system (100) according to claim 8, wherein in the first operational mode the one or more multiple-position valves (140) provide a sampling pump flow path (17) from the reactor (50) via the sampling compartment (150) back to the reactor (50), wherein the pump (170) is configured to control a sampling pump flow through the sampling pump flow path (17).

10. The system (100) according to claim 5, wherein the control system (300) is configured to control one or more of a gas pressure of inlet gas, a solvent supply pressure, a solvent compartment pressure, a sampling compartment pressure, and a reactor pressure.

11. A method for sampling from a reactor (50) using the sampling arrangement (105) according to claim 1, the method comprising consecutively executing the first operational mode (10) and the second operational mode (20), wherein the method further comprises providing an inlet gas from the gas inlet (110) during at least part of the second operational mode (20).

12. The method according to claim 11, wherein the method comprises switching between the first operational mode (10) and the second operational mode (20) using the one or more multiple-position valves (140).

13. The method according to claim 11, the method comprising: providing a lower pressure in the sampling compartment (150) than in the reactor (50) during at least part of the first operational mode (10); and/or providing during at least part of the first operational mode (10) a solvent at the solvent inlet (120) with a solvent pressure exceeding the pressure in the solvent compartment (130).

14. The method according to claim 11, wherein the method comprises providing the inlet gas at a pressure above atmospheric pressure, and wherein the inlet gas is an inert gas.

15. Use of the sampling arrangement according to claim 1 to sample from a reactor.

16. Use according to claim 15, wherein the reactor is under a controlled atmosphere.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0105] Embodiments of the invention will now be described, by way of example only, with reference to the accompanying schematic drawings in which corresponding reference symbols indicate corresponding parts, and in which: FIG. 1A-B schematically depict an embodiment of the sampling arrangement (105). FIG. 2 schematically depicts an embodiment of the system (100). The schematic drawings are not necessarily on scale.

DETAILED DESCRIPTION OF THE EMBODIMENTS

[0106] FIG. 1A-B schematically depict an embodiment of a sampling arrangement 105 for sampling from a reactor 50. The sampling arrangement 105 comprises a solvent compartment 130, one or more multiple-position valves 140, and a sampling compartment 150. The sampling arrangement may be configured operable in a first operational mode 10 and a second operational mode 20. In the depicted embodiments, the one or more multiple-position valves 140 comprises a 10-position valve, especially a 10-position two-way valve. The one or more multiple-position valves 140, especially the 10-position valve, are operable in a first configuration and in a second configuration, wherein the sampling arrangement 105 is in the first operational mode 10 when the one or more multiple-position valves 140 are in the first configuration, and wherein the sampling arrangement 105 is in the second operational mode 20 when the one or more multiple-position valves 140 are in the second configuration. The solid lines in FIG. 1A indicate fluid contacts between (adjacent) positions of the 10-position valve in the first configuration, and the solid lines in FIG. 1B indicate the fluid contacts between (adjacent) positions of the 10-position valve in the second configuration (FIG. 1B).

[0107] FIG. 1A depicts an embodiment of the sampling arrangement 105 in the first operational mode 10. In the first operational mode 10 the one or more multiple-position valves 140 are configured to provide: a fluid contact between a solvent inlet 120 and the solvent compartment 130; a fluid contact between the reactor 50 and the sampling compartment 150; and fluid separation between the solvent compartment 130 and the sampling compartment 150. In particular, in further embodiments, in the first operational mode 10 the one or more multiple position valves 140 may be configured to provide a solvent flow path 13 from the solvent inlet 120 to the solvent compartment 130. In further embodiments, in the first operational mode 10 the one or more multiple position valves 140 may be configured to provide a sampling flow path 15 from the reactor 50 to the sampling compartment 150.

[0108] In embodiments, the sampling arrangement 105 may further comprise or be functionally coupled to a pump 170, especially wherein in the first operational mode 10 the one or more multiple-position valves 140 are configured to provide a fluid contact between the pump 170, the sampling compartment 150 and the reactor 50. In further embodiments, in the first operational mode the one or more multiple-position valves 140 may provide a sampling pump flow path 17 from the reactor 50 via the sampling compartment 150 back to the reactor 50, especially wherein the pump 170 is configured to control a sampling flow through the sampling pump flow path 17. The sampling pump flow path 17 may especially comprise the sampling flow path 15.

[0109] FIG. 1B depicts an embodiment of the sampling arrangement 105 in the second operational mode 20. In the second operational mode 20 the one or more multiple-position valves 140 are configured to provide: fluid contact between (successively) a gas inlet 110, the solvent compartment 130, the sampling compartment 150, and an outlet 160.

[0110] In further embodiments, in the second operational mode 20 the one or more multiple-position valves 140 are configured to provide fluid separation between the solvent inlet 120 and the solvent compartment 130. In further embodiments, in the second operational mode 20 the one or more multiple-position valves 140 are configured to provide fluid separation between the sampling compartment 150 and the reactor 50.

[0111] In the depicted embodiment, the sampling arrangement 105 comprises a 10-position valve, wherein the 10-position valves comprises 10 positions (P.sub.1-P.sub.10), wherein: a first position P.sub.1 indicates a gas inlet position; a second position P.sub.2 indicates a solvent compartment inlet; a third position P.sub.3 indicates a solvent inlet position; a fourth position P.sub.4 indicates a solvent stop; a fifth position P.sub.5 indicates a solvent outlet position; a sixth position P.sub.6 indicates a sampling compartment inlet; a seventh position P.sub.7 indicates a reactor inlet position; an eighth position P.sub.8 indicates a sampling stop; a ninth position P.sub.9 indicates a sampling compartment outlet; and a tenth position P.sub.10 indicates an outlet position. Especially, in the first operational mode 10: P.sub.10 may be in fluid contact with P.sub.1; P.sub.2 may be in fluid contact with P.sub.3; P.sub.4 may be in fluid contact with P.sub.5; P.sub.6 may be in fluid contact with P.sub.7; and P.sub.8 may be in fluid contact with P.sub.9, and in the second operational mode 20: P.sub.1 may be in fluid contact with P.sub.2; P.sub.3 may be in fluid contact with P.sub.4; P.sub.5 may be in fluid contact with P.sub.6; P.sub.7 may be in fluid contact with P.sub.8; and P.sub.9 may be in fluid contact with P.sub.10.

[0112] In further embodiments, the first position P.sub.1 is functionally coupled to the gas inlet 110, the third position P.sub.3 is functionally coupled to the solvent inlet 120, the seventh position P.sub.7 is functionally coupled to the reactor 50, and the tenth position P.sub.10 is functionally coupled to the outlet. In further embodiments, the fourth position P.sub.4 may be functionally coupled to a blinding nut. Similarly, in further embodiments, the eighth position P.sub.8 may be functionally coupled to a blinding nut.

[0113] In further embodiments, the sampling compartment 150 may have a sampling volume V.sub.150 selected from the range of 50 μl-5 ml and the solvent compartment 130 may have a solvent volume V.sub.130≥2V.sub.150. The sampling volume may herein specifically refer to the total volume in between the respective connected positions (P.sub.6, P.sub.9) of the multi-position valve, i.e. it may refer to the volume of the sampling compartment 150 as well as the volume of any connected tubing. Essentially, however, the volume of the sampling compartment 150 primarily dictates the sampling volume. Further, it will be clear to the person skilled in the art that in many applications the exact available sampling volume may not directly dictate the volume of the sample. For example, a 50 μl loop used with sampling from a pressurized autoclave may not give exactly 50 μl of liquid. For example, prior to sampling the loop may be filled (with a gas) at a pressure of 1 atm, which may be compressed by an incoming liquid at an operating pressure (i.e., approx. to 1/50th of the volume at an operating pressure of 50 atm). It will further be clear to the person skilled in the art that a deviation in the exact sampling volume can be addressed in downstream analyses, particularly when an internal standard is used.

[0114] In the depicted embodiment, the sampling compartment 150 is (configured to be) arranged external to the reactor 50 during operation of the sampling arrangement 150. However, in further embodiments, the sampling compartment 150 may be (configured to be) arranged inside of the reactor 50 during operation of the sampling arrangement 150.

[0115] FIG. 2 schematically depicts an embodiment of the system 100 comprising the sampling arrangement 105. In the depicted embodiment, the system 100 further comprises a control system 300, wherein the control system 300 is configured to control the one or more multiple-position valves 140. In further embodiments, the control system may be configured to in a first mode of operation consecutively execute the first operational mode 10 and the second operational mode 20.

[0116] In the depicted embodiment, the system comprises or is functionally coupled to a gas supply 115, wherein the gas supply 115 is functionally coupled to the gas inlet 110.

[0117] In the depicted embodiment, the system 100 comprises or is functionally coupled to a solvent supply 125, wherein the solvent supply 125 is functionally coupled to the solvent inlet 120. Further, the system 100 comprises a solvent supply pressurizer 121 configured to pressurize the solvent supply 125 during the first operational mode 10. In the depicted embodiment, the solvent supply pressurizer 121 is functionally coupled to the gas supply 115, especially via a solvent supply valve 124. Especially, the gas supply 115 may be configured to provide a gas, especially the inlet gas, to pressurize the solvent in the solvent supply 125. In further embodiments, the solvent supply pressurizer 121 may (alternatively) be functionally coupled to a second gas supply.

[0118] The system 100, in the depicted embodiment, further comprises or is functionally coupled to a dispenser valve 164, wherein the dispenser valve 164 is functionally coupled to the outlet 160. The dispenser valve 164 may be configured to dispense fluid, especially the solvent portion and the sample, to an outlet container 60. In particular, the dispenser valve 164 may be configured to dispense successive samples (with corresponding solvent portions) to different outlet containers 60. In further embodiments, the control system 300 may be configured to control the dispenser valve 164.

[0119] In embodiments, the outlet container 60 may be a chromatography vial, especially a chromatography vial suitable for subsequent analysis, such as for GC or HPLC analysis.

[0120] In embodiments, the outlet container 60 may comprise a quenching agent configured to quench the sample upon being dispensed to the outlet container 60.

[0121] In further embodiments, the system 100 may further comprise a pump 170, especially wherein in the first operational mode 10 the one or more multiple-position valves 140 are configured to provide a fluid contact between the pump 170, the sampling compartment 150 and the reactor 50. In further embodiments, in the first operational mode the one or more multiple-position valves 140 provide a sampling pump flow path 17 from the reactor 50 via the sampling compartment 150 back to the reactor 50, especially wherein the pump 170 is configured to control a sampling flow through the sampling pump flow path 17.

[0122] In such embodiments, the method may in the first operational mode 10 comprise providing a sampling pump flow, especially along a sampling pump flow path 17, from the reactor 50 via the sampling compartment 150 to the reactor 50.

[0123] The system 100 may be configured to drive fluid based on pressure differences, i.e., the system may be configured for one or more of: (i) filling the sampling compartment 150 with a sample from the reactor 50 based on a pressure difference, (ii) filling the solvent compartment 130 with a solvent portion from the solvent inlet 120, especially the solvent supply 125, based on a pressure difference, and (iii) driving the solvent portion and the sample to the outlet 160 by providing a (pressurized) inlet gas from the gas inlet 110. Hence, in further embodiments, the control system 300 may be configured to control one or more of a gas pressure of inlet gas, a solvent supply pressure, a solvent compartment pressure, a sampling compartment pressure, and a reactor pressure.

[0124] FIG. 1A-B and FIG. 2 further schematically depict embodiments of the method for sampling from a reactor 50. The method may comprise consecutively executing the first operational mode 10 and the second operational mode 20. The method may further comprise providing an inlet gas from the gas inlet 110, especially from the gas supply 115, during at least part of the second operational mode 20.

[0125] In further embodiments, the method may comprise providing one or more flow paths. In further embodiments, in the first operational mode 10 the method may comprise providing a solvent flow, especially along a solvent flow path 13, from the solvent inlet 120, especially from the solvent supply 125, to the solvent compartment 130. In further embodiments, in the first operational mode 10 the method may comprise providing a sampling flow, especially along a sampling flow path 15, from the reactor 50 to the sampling compartment 150.

[0126] In further embodiments, the method may comprise providing a lower pressure in the sampling compartment 150 than in the reactor 50 during at least part of the first operational mode 10, especially such that the sampling compartment 150 is filled with a sample from the reactor 50. In further embodiments, the method may comprise providing during at least part of the first operational mode 10 a solvent at the solvent inlet 120, especially from the solvent supply 125, with a solvent pressure exceeding the pressure in the solvent compartment 130, especially such that the solvent compartment 130 is filled with a solvent portion from the solvent inlet 120, especially from the solvent supply 125.

[0127] In further embodiments, in the second operational mode 20 the method may comprise providing an outlet flow, especially along an outlet flow path 26, from the gas inlet 110, especially from the gas supply 115, via the solvent compartment 130 and the sampling compartment 150 to the outlet 160. In further embodiments, the method may comprise (during the second operational mode 20) providing the inlet gas at a pressure suitable to drive the solvent portion and the sample to the outlet 160, especially providing the inlet gas at a pressure above atmospheric pressure.

[0128] In embodiments, the method may comprise switching between the first operational mode 10 and the second operational mode 20 using the one or more multiple-position valves, especially using the 10-position valve.

[0129] FIG. 1A-B and FIG. 2 further depict a use of the sampling arrangement 105 according to sample from a reactor 50, wherein the reactor 50 is especially (operated) under a controlled atmosphere.

[0130] The term “plurality” refers to two or more. Furthermore, the terms “a plurality of” and “a number of” may be used interchangeably.

[0131] The terms “substantially” or “essentially” herein, and similar terms, will be understood by the person skilled in the art. The terms “substantially” or “essentially” may also include embodiments with “entirely”, “completely”, “all”, etc. Hence, in embodiments the adjective substantially or essentially may also be removed. Where applicable, the term “substantially” or the term “essentially” may also relate to 90% or higher, such as 95% or higher, especially 99% or higher, even more especially 99.5% or higher, including 100%. Moreover, the terms “about” and “approximately” may also relate to 90% or higher, such as 95% or higher, especially 99% or higher, even more especially 99.5% or higher, including 100%. For numerical values it is to be understood that the terms “substantially”, “essentially”, “about”, and “approximately” may also relate to the range of 90%-110%, such as 95%-105%, especially 99%-101% of the values(s) it refers to.

[0132] The term “comprise” includes also embodiments wherein the term “comprises” means “consists of”.

[0133] The term “and/or” especially relates to one or more of the items mentioned before and after “and/or”. For instance, a phrase “item 1 and/or item 2” and similar phrases may relate to one or more of item 1 and item 2. The term “comprising” may in an embodiment refer to “consisting of” but may in another embodiment also refer to “containing at least the defined species and optionally one or more other species”.

[0134] Furthermore, the terms first, second, third and the like in the description and in the claims, are used for distinguishing between similar elements and not necessarily for describing a sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances and that the embodiments of the invention described herein are capable of operation in other sequences than described or illustrated herein.

[0135] The devices, apparatus, or systems may herein amongst others be described during operation. As will be clear to the person skilled in the art, the invention is not limited to methods of operation, or devices, apparatus, or systems in operation.

[0136] The term “further embodiment” and similar terms may refer to an embodiment comprising the features of the previously discussed embodiment, but may also refer to an alternative embodiment.

[0137] It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design many alternative embodiments without departing from the scope of the appended claims.

[0138] In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim.

[0139] Use of the verb “to comprise” and its conjugations does not exclude the presence of elements or steps other than those stated in a claim. Unless the context clearly requires otherwise, throughout the description and the claims, the words “comprise”, “comprising”, “include”, “including”, “contain”, “containing” and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is to say, in the sense of “including, but not limited to”.

[0140] The article “a” or “an” preceding an element does not exclude the presence of a plurality of such elements.

[0141] The invention may be implemented by means of hardware comprising several distinct elements, and by means of a suitably programmed computer. In a device claim, or an apparatus claim, or a system claim, enumerating several means, several of these means may be embodied by one and the same item of hardware. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage.

[0142] The invention also provides a control system that may control the device, apparatus, or system, or that may execute the herein described method or process. Yet further, the invention also provides a computer program product, when running on a computer which is functionally coupled to or comprised by the device, apparatus, or system, controls one or more controllable elements of such device, apparatus, or system.

[0143] The invention further applies to a device, apparatus, or system comprising one or more of the characterizing features described in the description and/or shown in the attached drawings. The invention further pertains to a method or process comprising one or more of the characterizing features described in the description and/or shown in the attached drawings. Moreover, if a method or an embodiment of the method is described being executed in a device, apparatus, or system, it will be understood that the device, apparatus, or system is suitable for or configured for (executing) the method or the embodiment of the method respectively.

[0144] The various aspects discussed in this patent can be combined in order to provide additional advantages. Further, the person skilled in the art will understand that embodiments can be combined, and that also more than two embodiments can be combined. Furthermore, some of the features can form the basis for one or more divisional applications.