Laboratory system and method for sampling reactor contents

Abstract

A method of sampling a reaction liquid from a reactor wherein the method comprises the steps of:-bringing a sampling fluid connection into fluid communication with a secondary fluid channel inlet to form a first flow path extending from the sampling fluid connection to the secondary fluid channel inlet, and increasing the liquid level of the reaction liquid in the sample channel and increasing the pressure in the buffer volume of the sample channel by injecting a sampling fluid into the reactor via the first flow path and the secondary fluid channel inlet while sealing the buffer volume of the sample channel with respect to the secondary fluid connection and the exhaust gas connection, -drawing the sample into the sample channel,-bringing the secondary fluid connection into fluid communication with the sample extraction outlet, thereby forming a second flow path extending from the secondary fluid connection to the sample extraction outlet, and subsequently feeding a secondary fluid to the secondary fluid connection, thereby extracting the sample from the sample channel and moving it to a suitable destination. The invention also relates to a sample extraction device configured for extracting a sample from a reactor, for example using the above method, comprising:-a sample channel,-a secondary fluid channel,-a sample fluid connection,-a secondary fluid connection,-a sample extraction outlet,-an exhaust gas connection,-a buffer volume, the buffer volume is arranged between the sampling valve and the sampling fluid connection,-a valve system.

Description

Technical Field

[0001] The present invention relates to laboratory systems and sample extraction devices and methods, and in particular to at least partially automated laboratory systems and sample extraction devices and methods. Background Art

[0002] Particularly in process chemistry and crystallization analysis, many reactions are typically carried out in research. Sampling from such reactions is a valuable means for gaining insight into the reaction process such as crystallization and / or process chemistry. In current systems such as manual or partially automated pipetting devices, sampling is a labor-intensive and complex process, resulting in significant costs and possible human errors. In addition, current systems typically require relatively large samples to be taken.

[0003] Object of the Invention

[0004] The object of the present invention is to provide a device and method for sampling a reactor in an efficient manner. Another object of the present invention is to provide a device and method for sampling a reactor in an accurate and / or reproducible manner. Another object of the present invention is to provide a device and method for sampling a reactor in a less labor-intensive manner. Summary of the Invention

[0005] In order to achieve at least one of the objects, in a first aspect, there is provided a sample extraction device configured to extract a sample from a reactor, the sample extraction device comprising:

[0006] - a sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume,

[0007] - a secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0008] - a sampling fluid connection connected to the sample channel and configured to supply pressurized sampling fluid to the sample extraction device via the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen,

[0009] - a secondary fluid connection,

[0010] - a sample extraction outlet,

[0011] - an exhaust gas connection,

[0012] - a buffer volume disposed between the sampling valve and the sampling fluid connection,

[0013] - A valve system, which is connected to a sample channel, a secondary fluid channel, a sampling fluid connection, a secondary fluid connection, a sample extraction outlet, and an exhaust gas connection,

[0014] The valve system includes a sampling valve,

[0015] wherein:

[0016] - The sampling valve is arranged between the sampling fluid connection and the inlet of the sample channel,

[0017] - The sampling valve includes a sampling space having a cavity volume,

[0018] - The sampling valve is movable to a sampling position and is movable to a delivery position,

[0019] - In the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel,

[0020] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

[0021] The sample extraction device according to the present invention allows the reactor to be sampled in an effective manner, while minimizing the chance of operator error and providing high repeat accuracy. The valve system allows the formation of the required flow paths for performing various operations. The buffer volume prevents the over-entry of the sampled fluid into the system, thereby reducing the risk of contamination.

[0022] In an embodiment, the valve system can be arranged in a sampling configuration, wherein, in the sampling configuration:

[0023] - The sampling valve is in the sampling position,

[0024] - The inlet of the secondary fluid channel is in fluid communication with the sampling fluid connection,

[0025] - The inlet of the sample channel is not in fluid communication with the exhaust gas connection.

[0026] In an embodiment, the valve system includes a sample blocking valve, which is arranged in the sample channel, between the sampling valve and the sampling fluid connection, wherein the sample blocking valve is arranged in the blocking position in the sampling configuration of the valve system.

[0027] The sample blocking valve prevents the sampled fluid from passing through during sampling and / or causes a pressure rise in the sample channel during sampling. The pressure in the buffer volume is opposite to the pressure in the reactor volume. This helps to control the sampling process and the liquid level of the sampled fluid in the sample channel. The sample blocking valve can be in the passing position in cases other than during sampling and / or can be opened in some cases other than during sampling.

[0028] In an embodiment, a buffer volume is arranged between the sampling valve and the sample blocking valve.

[0029] In an embodiment, the valve system can be arranged in a pressure reduction configuration, wherein, in the pressure reduction configuration:

[0030] - The sampling valve is in the sampling position,

[0031] - The secondary fluid channel inlet is in fluid communication with the exhaust gas,

[0032] - The sample channel inlet is in fluid communication with the exhaust gas.

[0033] In an embodiment, the valve system can be arranged in a delivery configuration, wherein, in the delivery configuration:

[0034] - The sampling valve is in the delivery position,

[0035] - The secondary fluid connection is in fluid communication with the sampling space.

[0036] Since the sampling space is in fluid communication with the secondary fluid connection, the secondary fluid connection can be used to provide fluid to move the sample from the sampling space to a suitable location.

[0037] In an embodiment, in the delivery configuration:

[0038] - The sample extraction outlet is in fluid communication with the secondary fluid connection, and / or

[0039] - The sample channel inlet is not in fluid communication with the sampling fluid connection.

[0040] Since the sample extraction outlet is in fluid communication with the secondary fluid connection, the secondary fluid connection can be used to provide fluid to move the sample from the sampling space to a suitable location via the sample extraction outlet.

[0041] In an embodiment:

[0042] - The secondary fluid connection includes a delivery fluid connection for providing a delivery fluid, wherein, optionally, the delivery fluid is an inert gas, preferably nitrogen,

[0043] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the delivery fluid connection.

[0044] In an embodiment, the sample extraction device includes a cleaning fluid connection, wherein the valve system can be arranged in a cleaning configuration, wherein, optionally, the cleaning fluid connection is the sampling fluid connection, wherein, in the cleaning configuration:

[0045] - The cleaning fluid connection is in fluid communication with the sample channel inlet,

[0046] - The secondary fluid channel inlet is in fluid communication with the exhaust gas.

[0047] In a cleaning configuration, fluid can be directed from a cleaning fluid connection through a sample channel into a reactor to clean and / or wash the sample channel.

[0048] In an embodiment:

[0049] - The secondary fluid connection includes a quench fluid connection for providing quench fluid,

[0050] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the quench fluid connection.

[0051] The quench fluid can stop one or more chemical reactions occurring in the sample.

[0052] In an embodiment:

[0053] - The secondary fluid connection includes a dilution fluid connection for providing dilution fluid,

[0054] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the dilution fluid connection.

[0055] The dilution fluid can dilute the sample to make it suitable for analysis.

[0056] In an embodiment, the sampling valve is configured to be disposed above the liquid level of the reaction liquid in the reactor volume.

[0057] In an embodiment, the sample extraction device includes a valve system, and the valve system includes:

[0058] - A secondary fluid valve disposed in the secondary fluid channel and between the secondary fluid connection and the secondary fluid channel inlet,

[0059] Wherein:

[0060] - The secondary fluid valve can move to a secondary blocking position, wherein the secondary fluid valve blocks the flow through the secondary fluid channel such that the flow through the secondary fluid channel inlet is blocked, and the secondary fluid valve can move to a secondary flow position, wherein the secondary fluid valve allows the flow through the secondary fluid channel and allows the flow through the secondary fluid channel inlet.

[0061] In a second aspect of the present invention, a method for sampling reaction liquid from a reactor is provided, the method comprising the steps of:

[0062] - Providing a sample extraction device including the features of the foregoing embodiments,

[0063] - Fluidly connect the sampling fluid connection to the secondary fluid channel inlet to form a first flow path extending from the sampling fluid connection to the secondary fluid channel inlet, and inject the sampling fluid into the reactor via the first flow path and the secondary fluid channel inlet while sealing the buffer volume of the sample channel relative to the secondary fluid connection and the exhaust connection, thereby raising the liquid level of the reaction liquid in the sample channel and increasing the pressure in the buffer volume of the sample channel, and drawing the sample into the sample channel.

[0064] - Fluidly connect the secondary fluid connection to the sample extraction outlet, thereby forming a second flow path extending from the secondary fluid connection to the sample extraction outlet, and subsequently feed the secondary fluid to the secondary fluid connection, thereby extracting the sample from the sample channel and moving it to a suitable destination.

[0065] Since the buffer volume is sealed relative to the secondary fluid connection and the exhaust connection during sampling, the pressure in the buffer volume will increase as the sampling fluid is injected into the reactor and the liquid level of the reaction liquid rises in the sample channel. This rising pressure counteracts the pressure in the reactor that forces the reaction liquid into the sample channel. In this way, the liquid level of the reaction liquid in the sample channel is controlled.

[0066] In an embodiment, the method includes the steps of: depressurizing the volume in the sample channel, the volume in the secondary fluid channel, and the reactor volume by arranging a valve system to fluidly connect the sample channel and the secondary fluid channel to the exhaust connection, thereby forming a third flow path extending from the secondary fluid channel inlet to the exhaust connection and a fourth flow path extending from the sample channel inlet to the exhaust connection.

[0067] The depressurization step ensures that the pressure at points in the system is known and substantially equal to the pressure of the exhaust connection. This allows for accurate control of the system during sampling.

[0068] In an embodiment, the depressurization step includes arranging the valve system in a depressurized configuration.

[0069] In an embodiment, the method includes the step of cleaning the sample extraction device by:

[0070] - Injecting a cleaning fluid from the sampling fluid connection into the reactor volume via the sample channel, thereby blowing any reaction liquid out of the sample channel, where optionally, the cleaning fluid is an inert gas such as nitrogen.

[0071] - Removing the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection.

[0072] - wherein the step of cleaning the sample extraction device is preferably performed before sampling the sample.

[0073] During cleaning, fluid is directed through the sample channel into the reactor to clean and / or wash the sample channel. Additionally, as the reaction liquid is pushed out of the sample channel, a fresh, well-mixed sample can then be taken from the reactor rather than a sample that has resided in the sample channel for a longer period of time.

[0074] In an embodiment, the step of cleaning the sample extraction device includes arranging the valve system in a cleaning configuration.

[0075] In an embodiment, the method includes flushing the sampling tube by performing the following steps:

[0076] - Injecting a sampling fluid into the reactor volume via the secondary fluid channel inlet, thereby raising the level of the reaction liquid in the sample channel,

[0077] - Subsequently, removing fluid from the reactor volume via the secondary fluid channel inlet, thereby lowering the level of the reaction liquid in the sample channel,

[0078] - Optionally repeating the steps of injecting and removing the sampling fluid via the secondary fluid channel inlet,

[0079] wherein the steps are preferably performed before depressurizing and sampling the sample.

[0080] Injecting the sampling fluid and subsequently removing fluid from the reactor via the secondary fluid channel inlet alternately raises and lowers the level of the reaction liquid in the sample channel. This helps to clean the sample channel.

[0081] In an embodiment, the step of sampling the sample includes arranging the valve system in a sampling configuration.

[0082] In an embodiment, the step of sampling the sample includes the following steps:

[0083] - Injecting a sampling fluid into the reactor volume via the sampling fluid connection, valve system, and secondary fluid channel inlet, thereby forcing the reaction liquid from the reactor volume into the sample channel, through and past the sampling valve, and into the buffer volume of the sample channel,

[0084] - Adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume to control the level of the reaction liquid in the buffer volume.

[0085] By adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume, the level of the reaction liquid in the buffer volume can be controlled. Preferably, the pressure of the sampling fluid is controlled such that when the reaction liquid is at the desired level in the buffer volume, the pressure of the sampling fluid is similar to the expected backpressure caused by the sealing of the buffer volume.

[0086] In an embodiment, the step of extracting a sample and moving it to a suitable location includes arranging a valve system in a delivery configuration.

[0087] In an embodiment, the secondary fluid includes a quench fluid and / or a dilution fluid and / or a delivery fluid, and the delivery fluid is preferably an inert gas such as nitrogen.

[0088] The quench fluid can stop one or more chemical reactions occurring in the sample. The dilution fluid can dilute the sample to make it suitable for analysis. Alternatively or in addition to the quench fluid and / or the dilution fluid, a delivery fluid can be used.

[0089] In a third aspect of the present invention, there is provided a laboratory system comprising:

[0090] - at least one reactor,

[0091] - a sample extraction device for extracting a sample from at least one reactor into a sampling space,

[0092] - a fluid supply system including a delivery fluid supply device,

[0093] - at least one sample storage container,

[0094] - at least one fluid supply channel connecting the extraction device to the fluid supply system,

[0095] - at least one sample extraction channel connecting the extraction device to the sample storage container,

[0096] wherein the fluid supply system is arranged to use the delivery fluid of the delivery fluid supply device to push the sample from the sampling space through the sample extraction channel to at least one sample storage container.

[0097] The system according to the present invention allows sampling of the reactor in an efficient manner, while minimizing the chance of operator error and providing high repeat accuracy. The sample extraction device can be any sample extraction device, such as the sample extraction device according to one of the first aspect, the fifth aspect, the seventh aspect or the eleventh aspect.

[0098] In an embodiment of the laboratory system, the laboratory system comprises:

[0099] - a plurality of sample storage containers,

[0100] - a container selection system for associating at least one sample extraction channel with one of the plurality of sample storage containers.

[0101] In an embodiment of the laboratory system:

[0102] - The laboratory system includes multiple reactors,

[0103] - The sample extraction device cooperates with each of the multiple reactors via a downstream reactor selection system for extracting a sample from the selected reactor into a sampling space,

[0104] - At least one fluid supply channel connects the fluid supply system to the sample extraction device, and

[0105] - At least one sample extraction channel connects the sample extraction device to at least one sample storage container.

[0106] In an embodiment of the laboratory system, the laboratory system includes N reactors, wherein the downstream reactor selection system includes a downstream N-way valve configured to fluidly connect the sample extraction device to one of the N reactors. The downstream N-way valve includes one inlet and N outlets, creating a total of N + 1 fluid connections.

[0107] In an embodiment of the laboratory system:

[0108] - The laboratory system includes multiple reactors and multiple sample extraction devices,

[0109] - Each sample extraction device has a sampling space, and each sample extraction device cooperates with one of the multiple reactors for extracting a sample from at least one reactor into the corresponding sampling space,

[0110] - At least one fluid supply channel connects the fluid supply system to each sample extraction device, and

[0111] - At least one sample extraction channel connects each sample extraction device to at least one sample storage container.

[0112] In an embodiment of the laboratory system, the laboratory system includes N reactors, and the laboratory system includes an upstream reactor selection system configured to fluidly connect the sample extraction device of one of the N reactors to the fluid supply system. The upstream N-way valve includes one inlet and N outlets, creating a total of N + 1 fluid connections.

[0113] In an embodiment of the laboratory system, the upstream reactor selection system includes an upstream N-way valve arranged in the fluid supply channel.

[0114] In an embodiment of the laboratory system, at least one reactor is a thermal cycling reactor.

[0115] In an embodiment of the laboratory system, the fluid supply system includes a quench fluid supply device.

[0116] In an embodiment of the laboratory system, the fluid supply system is arranged to use the conveying fluid of the conveying fluid supply device to push the quenching fluid from the quenching fluid supply device through the fluid supply channel, the sampling space, and / or the sample extraction channel.

[0117] In an embodiment of the laboratory system, the fluid supply system includes a dilution fluid supply device.

[0118] In an embodiment of the laboratory system, the fluid supply system is arranged to use the conveying fluid of the conveying fluid supply device to push the dilution fluid from the dilution fluid supply device through the fluid supply channel, the sampling space, and / or the sample extraction channel.

[0119] In an embodiment of the laboratory system, the fluid supply system includes a flushing fluid supply device.

[0120] In an embodiment of the laboratory system, the fluid supply system is arranged to use the conveying fluid of the conveying fluid supply device to push the flushing fluid from the flushing fluid supply device through the fluid supply channel, the sampling space, and / or the sample extraction channel.

[0121] In an embodiment of the laboratory system, the sample extraction device includes:

[0122] - A sample channel configured to extend into the reactor volume of the reactor. The sample channel includes a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume of the reactor.

[0123] - A sampling valve disposed in the sample channel and including a sampling space. The sampling valve is movable between a sampling position and a conveying position.

[0124] - A secondary fluid channel configured to extend into the reactor volume of the reactor. The secondary fluid channel includes a secondary fluid channel inlet.

[0125] Wherein, in the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel, and wherein, in the conveying position of the sampling valve, the sampling space is in fluid communication with at least one fluid supply channel and at least one sample extraction channel.

[0126] In an embodiment of the laboratory system, the secondary fluid channel can be connected to the conveying fluid supply device.

[0127] In a fourth aspect, the present invention provides a method of sampling using a laboratory system according to any embodiment of the embodiments in the third aspect. The method includes the following steps:

[0128] - Extract the sample from the reactor into the sampling space.

[0129] - Transport the sample via the sample extraction channel to the sample storage container by supplying a transport fluid via the fluid supply channel to the sampling space.

[0130] In an embodiment of the sampling method, the method includes the step of supplying a quenching fluid from a quenching fluid supply device to the sample.

[0131] In an embodiment of the sampling method, supply the quenching fluid to the sample via the fluid supply channel.

[0132] In an embodiment of the sampling method, supply the quenching fluid to the sample in the sample storage container.

[0133] In an embodiment of the sampling method, the step of supplying the quenching fluid includes: using the transport fluid of the transport fluid supply device to push the quenching fluid through the fluid supply channel, the sampling space, and / or the sample extraction channel.

[0134] In an embodiment of the sampling method, the method includes the step of supplying a dilution fluid to the sample.

[0135] In an embodiment of the sampling method, supply the dilution fluid to the sample via the fluid supply channel.

[0136] In an embodiment of the sampling method, supply the dilution fluid to the sample in the sample storage container.

[0137] In an embodiment of the sampling method, the step of supplying the dilution fluid includes: using the transport fluid of the transport fluid supply device to push the dilution fluid through the fluid supply channel, the sampling space, and / or the sample extraction channel.

[0138] In an embodiment of the sampling method, the method includes a flushing step of flushing the fluid supply channel by supplying a flushing fluid from a flushing fluid supply device to the fluid supply channel and depositing the flushing fluid in the waste container.

[0139] In an embodiment of the sampling method, the flushing step further includes: flushing the sampling space and / or at least one sample extraction channel by supplying the flushing fluid from the fluid supply channel to the sampling space and / or at least one sample extraction channel.

[0140] In an embodiment of the sampling method, the step of supplying the flushing fluid includes: using the transport fluid of the transport fluid supply device to push the flushing fluid through the fluid supply channel, the sampling space, and / or the sample extraction channel.

[0141] In an embodiment of the sampling method, extract the sample from the reactor into the sampling space by injecting the transport fluid via a secondary fluid channel into the reactor volume.

[0142] In an embodiment of the sampling method, the method includes the step of registering a sample trigger to initiate sampling. The sample trigger may include a timestamp, a temperature measurement falling within or outside a certain range, a measurement of a reactor process parameter such as a crystallization parameter, a transmittance measurement, a user input, or any other trigger. The measurements for determining the sample trigger may be performed by an analysis system including a Raman spectrometer and / or a camera device that monitors the reactor. Then, the timestamped data from the analysis system may be compared with the timestamped sample analysis data, such as data obtained by high performance liquid chromatography or any other offline analysis of the sample, in order to obtain a comprehensive data set of the reactor process.

[0143] In a fifth aspect, the present invention provides a sample extraction device configured to extract a sample from a reactor, the sample extraction device including:

[0144] - a sample extraction outlet,

[0145] - a sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume of the reactor,

[0146] - a sampling valve disposed in the sample channel,

[0147] - a secondary fluid channel configured to extend into the reactor volume of the reactor, the secondary fluid channel including a secondary fluid channel inlet,

[0148] wherein:

[0149] - the sampling valve includes a sampling space having a cavity volume,

[0150] - the sampling valve is movable between a sampling position and a delivery position,

[0151] wherein, in the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel, and wherein, in the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

[0152] The sample extraction device according to the present invention allows for the extraction of a sample from a reactor in an efficient manner, while minimizing the chance of operator error and providing high repeat accuracy.

[0153] In a sixth aspect, the present invention provides a method of sampling reaction liquid from a reactor using the sample extraction device according to the previous embodiment, the method including the steps of:

[0154] - disposing the sampling valve in the sampling position,

[0155] - Filling the sampling space with a sampling volume of the reaction liquid via the sample channel, the sampling volume being equal to the chamber volume,

[0156] - Subsequently arranging the sampling valve in the delivery position,

[0157] - Delivering the sampling volume of the reaction liquid from the sampling space through the sample extraction outlet to a suitable destination.

[0158] In an embodiment of the sampling method, the step of filling the sampling space is performed by applying a pressure difference between the reactor volume and the sampling space.

[0159] In an embodiment of the sampling method, the pressure difference is achieved by introducing a fluid via the secondary fluid channel into the reactor volume at a pressure higher than the pressure in the sampling space, thereby forcing the reaction liquid through the sample channel into the sampling space.

[0160] In a seventh aspect, the present invention provides a sample extraction device configured to extract a sample from a reactor, the sample extraction device comprising:

[0161] - A sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume,

[0162] - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0163] - A sampling fluid connection connected to the sample channel, the sampling fluid connection being configured to supply pressurized sampling fluid to the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen,

[0164] - A secondary fluid connection connected to the secondary fluid channel,

[0165] - A sampling three-way valve disposed in the sample channel, the sampling three-way valve including a first sampling connection, a second sampling connection, and a third sampling connection, wherein the first sampling connection and the second sampling connection are connected in series with the sampling channel, and wherein the third sampling connection is connected to a sampling cross-tube that is connected to the secondary fluid channel at a secondary cross-connection, wherein the first sampling connection is disposed between the second sampling connection and the sampling fluid connection, and the second sampling connection is disposed between the first sampling connection and the sample channel inlet,

[0166] Wherein:

[0167] - The sampling three-way valve is arranged between the sampling fluid connection and the sample channel inlet.

[0168] - The sampling three-way valve can be moved to a sampling in-line through position, wherein fluid flow between the first sampling connection and the second sampling connection is allowed, and wherein fluid flow through the third sampling connection is not allowed.

[0169] - The sampling three-way valve can be moved to a first sampling cross position, wherein fluid flow between the first sampling connection and the third sampling connection is allowed, and wherein fluid flow through the second sampling connection is not allowed.

[0170] This sample extraction device allows for effective, accurate, and highly repeatable sampling of the reaction liquid from the reactor.

[0171] In an embodiment of the sample extraction device, the secondary fluid channel inlet is configured to be positioned above the liquid level of the reaction liquid in the reactor volume.

[0172] In an embodiment of the sample extraction device, the sample extraction device is incorporated into a cap that can be attached to a reactor vessel in a standard format.

[0173] In an embodiment of the sample extraction device, optionally, the sample extraction device can be connected to a port on the laboratory system chassis without an external tube (e.g., via a click-connection system).

[0174] In an embodiment of the sample extraction device, the sample extraction device includes:

[0175] - A sampling valve, the sampling valve is arranged in the sample channel.

[0176] - A sample extraction outlet.

[0177] Wherein:

[0178] - The sampling valve is arranged between the sampling fluid connection and the sample channel inlet, wherein the sampling valve is preferably arranged between the sampling three-way valve and the sample channel inlet.

[0179] - The sampling valve includes a sampling space having a cavity volume.

[0180] - The sampling valve can be moved to a sampling position and a delivery position.

[0181] - In the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel.

[0182] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

[0183] In an embodiment of the sample extraction device, the sample extraction device includes:

[0184] - For providing a fluid conveyance connection for conveying a fluid, wherein, optionally, the conveying fluid is an inert gas, preferably nitrogen,

[0185] - At the conveyance position of the sampling valve, the sampling space is in fluid communication with the fluid conveyance connection at the conveyance position of the sampling valve.

[0186] In an embodiment of the sample extraction device, the sampling valve is configured to be arranged above the liquid level of the reaction liquid in the reactor volume.

[0187] In an embodiment of the sample extraction device, the sample channel includes a buffer volume arranged between the sampling valve and the sampling fluid connection, wherein the buffer volume is preferably arranged between the sampling valve and the sampling three-way valve.

[0188] In an embodiment of the sample extraction device, the sample extraction device includes:

[0189] - A secondary fluid valve, the secondary fluid valve being arranged in the secondary fluid channel and between the secondary fluid connection and the secondary fluid channel inlet, wherein the secondary fluid valve is preferably arranged between the secondary cross-connection and the secondary fluid channel inlet,

[0190] Wherein:

[0191] - The secondary fluid valve can be moved to a secondary blocking position, wherein the secondary fluid valve blocks the flow through the secondary fluid channel, and the secondary fluid valve can be moved to a secondary flow position, wherein the secondary fluid valve allows the flow through the secondary fluid channel.

[0192] In an embodiment of the sample extraction device, the sample extraction device includes:

[0193] - A secondary three-way valve arranged in the secondary fluid channel, the secondary three-way valve including a first secondary connection, a second secondary connection and a third secondary connection, wherein the first secondary connection and the second secondary connection are connected in series with the secondary fluid channel, and wherein the third secondary connection is connected to a secondary cross pipe, the secondary cross pipe being connected to the sample channel at the sampling cross-connection, wherein the first secondary fluid connection is arranged between the second secondary fluid connection and the secondary fluid connection, and the second secondary fluid connection is arranged between the first secondary fluid connection and the secondary fluid channel inlet,

[0194] Wherein:

[0195] - The secondary three-way valve is arranged between the secondary fluid connection and the secondary fluid channel inlet, wherein the secondary three-way valve is preferably arranged between the secondary fluid connection and the secondary cross-connection,

[0196] - The secondary three-way valve is movable to a secondary in-line through position, wherein fluid flow between a first secondary connection and a second secondary connection is permitted and wherein fluid flow through a third secondary connection is not permitted.

[0197] - The secondary three-way valve is movable to a first secondary cross position, wherein fluid flow between a first secondary connection and a third secondary connection is permitted and wherein fluid flow through a second secondary connection is not permitted.

[0198] In an embodiment of the sample extraction device:

[0199] - The secondary cross-connection is arranged between the secondary three-way valve and the secondary fluid valve.

[0200] In an embodiment of the sample extraction device:

[0201] - The sampling cross-connection is arranged between the sampling three-way valve and the sampling valve.

[0202] In an embodiment of the sample extraction device, the sample extraction device comprises:

[0203] - A sampling two-way valve arranged in the sample channel, between the sampling fluid connection and the sampling three-way valve, wherein the sampling two-way valve is movable to a sampling open position permitting flow through the sampling two-way valve and a sampling closed position not permitting flow through the sampling two-way valve, and / or

[0204] - A secondary two-way valve arranged in the secondary fluid channel, between the secondary fluid connection and the secondary three-way valve, wherein the secondary two-way valve is movable to a secondary open position permitting flow through the secondary two-way valve and a secondary closed position not permitting flow through the secondary two-way valve.

[0205] In an eighth aspect, the present invention provides a method of sampling reaction liquid from a reactor using a sample extraction device, the sample extraction device comprising:

[0206] - A sample channel configured to extend into the reactor volume of the reactor, the sample channel comprising a sample channel inlet configured to be arranged below the liquid level of the reaction liquid in the reactor volume,

[0207] - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel comprising a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0208] - A sampling fluid connection connected to the sample channel, the sampling fluid connection being configured to supply pressurized sampling fluid to the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen,

[0209] - A secondary fluid connection that connects to a secondary fluid passage

[0210] wherein the method comprises the steps of:

[0211] - Depressurizing the volume in the sample passage, the volume in the secondary fluid passage, and the reactor volume by fluidly connecting the sample passage and the secondary fluid passage to an exhaust gas region such as the atmosphere

[0212] - Injecting a sampling fluid into the reactor via the secondary fluid passage inlet while sealing the volume of the sample passage relative to the sampling fluid connection and the secondary fluid connection, thereby raising the liquid level of the reaction liquid in the sample passage and raising the pressure in the volume of the sample passage, and drawing a sample into the sample passage

[0213] - Extracting the sample from the sample passage and moving it to a suitable destination.

[0214] In an embodiment of the sampling method, the method comprises the steps of:

[0215] - Injecting a cleaning fluid from the sampling fluid connection through the sample passage into the reactor volume, thereby blowing any reaction liquid out of the sample passage, wherein optionally the cleaning fluid is an inert gas such as nitrogen

[0216] - Removing the cleaning fluid from the reactor volume via the secondary fluid passage and the secondary fluid connection

[0217] wherein the steps are preferably performed before depressurizing and drawing the sample.

[0218] In an embodiment of the sampling method, the method comprises the steps of:

[0219] - Injecting a sampling fluid into the reactor volume via the secondary fluid passage inlet, thereby raising the liquid level of the reaction liquid in the sample passage

[0220] - Subsequently, removing fluid from the reactor volume via the secondary fluid passage inlet, thereby lowering the liquid level of the reaction liquid in the sample passage

[0221] wherein the steps are preferably performed before depressurizing and drawing the sample.

[0222] In an embodiment, the method comprises the steps of:

[0223] - Arranging a sampling three-way valve in a first sampling cross position

[0224] - Injecting a sampling fluid into the reactor volume via the sampling fluid connection, the sampling three-way valve, and the secondary fluid passage inlet, thereby raising the liquid level of the reaction liquid in the sample passage

[0225] - Subsequently, fluid is removed from the reactor volume via the sampling fluid connection, the sampling three-way valve, and the secondary fluid channel inlet, thereby reducing the liquid level of the reaction liquid in the sample channel.

[0226] Instead of using the sampling fluid, a different fluid can be used to flush the sample extraction device.

[0227] In an embodiment, the method includes the following steps:

[0228] - Close the sampling fluid connection and open the secondary fluid connection.

[0229] - Arrange the sampling three-way valve in the first sampling cross position.

[0230] - Arrange the secondary three-way valve alternately in the secondary in-line through position and the first secondary cross position multiple times to equalize the pressures in both the reactor volume and the sample channel with the pressure of the secondary fluid connection.

[0231] In an embodiment of the pressure reduction method, the step of reducing the pressure of the sample extraction device is performed before taking a sample from the reactor.

[0232] In an embodiment of the pressure reduction method, the method includes the step of arranging the sampling valve in the sampling position.

[0233] In an embodiment of the pressure reduction method, the method includes the step of arranging the secondary fluid valve in the secondary flow position.

[0234] In an embodiment, the method includes the following steps:

[0235] - Arrange the sampling three-way valve in the first sampling cross position.

[0236] - Arrange the sampling valve in the sampling position.

[0237] - Close the secondary fluid connection.

[0238] - Inject the sampling fluid into the reactor volume via the sampling fluid connection, the sampling three-way valve, and the secondary fluid channel inlet, thereby forcing the reaction liquid from the reactor volume into the sample channel and into the sampling space, thereby filling the sampling space with the sampling volume of the reaction liquid, where the sampling volume is equal to the cavity volume.

[0239] - Subsequently arrange the sampling valve in the delivery position.

[0240] - Deliver the sampling volume of the reaction liquid from the sampling space through the sample extraction outlet to a suitable destination.

[0241] In an embodiment of the sampling method, during injection of the sampling fluid into the reactor volume, the volume in the sample channel is sealed relative to the sampling fluid connection and the secondary fluid connection such that the pressure in the volume of the sample channel is increased by forcing reaction liquid from the reactor volume into the sample channel.

[0242] In an embodiment of the sampling method, the method comprises the steps of:

[0243] - Arranging a sampling three-way valve in a first sampling cross position,

[0244] - Injecting the sampling fluid into the reactor volume via the sampling fluid connection, the sampling three-way valve and the secondary fluid channel inlet, thereby forcing reaction liquid from the reactor volume into the sample channel, through and past the sampling valve, and into the buffer volume,

[0245] - Adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume to control the level of the reaction liquid in the buffer volume.

[0246] In an embodiment of the sampling method, the method comprises the steps of:

[0247] - Controlling the level of the reaction liquid in the buffer volume by adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume, thereby preventing the reaction liquid forced into the sample channel from reaching the sampling three-way valve.

[0248] In an embodiment of the sampling method, the pressure of the sampling fluid is controlled such that the sample in the sample channel rises completely through the sampling valve without undercharging or overshooting the sampling valve and contaminating the system. Optionally, when viewed from the reactor volume, the volume passing through the sampling valve is sealed relative to any volume via any path other than through the sampling valve.

[0249] In an embodiment of the sampling method, the pressure and volume of the sampling fluid injected into the reactor volume are selected such that, within the desired ranges of the density, viscosity and amount of the reaction liquid, the sample completely fills the sampling valve without undercharging or overshooting the sampling valve and contaminating the system.

[0250] In an embodiment of the sampling method, the method comprises performing the steps of:

[0251] - Before injecting the sampling fluid into the reactor volume, arranging the secondary fluid valve in a secondary flow position.

[0252] In an embodiment of the sampling method, the method comprises the steps of:

[0253] - After filling the sampling space with the sampling volume of the reaction liquid, the secondary fluid valve is arranged in the secondary blocking position.

[0254] In an embodiment, the method includes the steps of: before collecting a sample from the reactor:

[0255] - Arranging the sampling three-way valve in the sampling in-line through position,

[0256] - Arranging the secondary three-way valve in the secondary in-line through position,

[0257] - Injecting a cleaning fluid from the sampling fluid connection through the sample channel into the reactor volume, thereby blowing any reaction liquid out of the sample channel, wherein, optionally, the cleaning fluid is an inert gas such as nitrogen,

[0258] - Removing the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection.

[0259] In a ninth aspect, the present invention provides a method for sampling a reaction liquid according to any of the foregoing embodiments of any method aspect (i.e., the sixth aspect or the eighth aspect), wherein the method is performed using a device or system according to any aspect of the third aspect, the fourth aspect, the fifth aspect, or the seventh aspect.

[0260] In a tenth aspect, the present invention provides a method for sampling a reaction liquid, the method combining the steps of at least two of the foregoing embodiments of any method aspect (i.e., any aspect of the sixth aspect, the eighth aspect, or the ninth aspect).

[0261] In an eleventh aspect, the present invention provides a sample extraction device configured to extract a sample from a reactor, the sample extraction device including:

[0262] - A sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume,

[0263] - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0264] - A sampling fluid connection connected to the sample channel, the sampling fluid connection being configured to supply a pressurized sampling fluid to the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen,

[0265] - A secondary fluid connection connected to the secondary fluid channel,

[0266] - Multiport valve, wherein the multiport valve is connected in series with the sample channel via a first multiport connection and a second multiport connection, and wherein the multiport valve is connected in series with the secondary fluid channel via a third multiport connection and a fourth multiport connection,

[0267] wherein,

[0268] - The first multiport connection is arranged between the second multiport connection and the sampling fluid connection, the second multiport connection is arranged between the first multiport connection and the sample channel inlet, the third multiport connection is arranged between the fourth multiport connection and the secondary fluid connection, and the fourth multiport connection is arranged between the third multiport connection and the secondary fluid channel inlet,

[0269] The multiport valve can be configured to connect any one of the four multiport connections to one or more of the other multiport connections.

[0270] In an embodiment of the sample extraction device, the sample extraction device includes:

[0271] - Sampling valve, the sampling valve is arranged in the sample channel,

[0272] - Sample extraction outlet,

[0273] wherein:

[0274] - The sampling valve is arranged between the sampling fluid connection and the sample channel inlet, and preferably, the sampling valve is arranged between the multiport valve and the sample channel inlet,

[0275] - The sampling valve includes a sampling space having a cavity volume,

[0276] - The sampling valve can move to a sampling position and a delivery position,

[0277] - In the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel,

[0278] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

[0279] In an embodiment of the sample extraction device, the sample extraction device includes:

[0280] - Delivery fluid connection for providing a delivery fluid, wherein optionally, the delivery fluid is an inert gas, preferably nitrogen,

[0281] - At the delivery position of the sampling valve, the sampling space is in fluid communication with the delivery fluid connection at the delivery position of the sampling valve.

[0282] In an embodiment of the sample extraction device, the sampling valve is configured to be arranged above the liquid level of the reaction liquid in the reactor volume.

[0283] In an embodiment of the sample extraction device, the sample channel includes a buffer volume arranged between the sampling valve and the sampling fluid connection, wherein the buffer volume is preferably arranged between the sampling valve and the multi-way valve.

[0284] In an embodiment of the sample extraction device, the sample extraction device includes:

[0285] - a secondary fluid valve arranged in the secondary fluid channel and between the secondary fluid connection and the secondary fluid channel inlet, wherein the secondary fluid valve is preferably arranged between the multi-way valve and the secondary fluid channel inlet,

[0286] wherein:

[0287] - the secondary fluid valve is movable to a secondary blocking position, wherein the secondary fluid valve blocks the flow through the secondary fluid channel, and the secondary fluid valve is movable to a secondary flow position, wherein the secondary fluid valve allows the flow through the secondary fluid channel.

[0288] In an embodiment of the sample extraction device, the sample extraction device includes:

[0289] - a sampling two-way valve arranged in the sample channel, between the sampling fluid connection and the sampling valve, wherein the sampling two-way valve is movable to a sampling open position allowing flow through the sampling two-way valve and a sampling closed position not allowing flow through the sampling two-way valve, and / or

[0290] - a secondary two-way valve arranged in the secondary fluid channel, between the secondary fluid connection and the secondary fluid valve, wherein the secondary two-way valve is movable to a secondary open position allowing flow through the secondary two-way valve and a secondary closed position not allowing flow through the secondary two-way valve.

[0291] In an embodiment, the method includes the following steps:

[0292] - arranging the multi-way valve to allow fluid flow between the first multi-way connection and the fourth multi-way connection and block the fluid flow through the second multi-way connection,

[0293] - injecting the sampling fluid into the reactor volume via the sampling fluid connection, the multi-way valve, and the secondary fluid channel inlet, thereby raising the liquid level of the reaction liquid in the sample channel,

[0294] - subsequently removing fluid from the reactor volume via the sampling fluid connection, the multi-way valve, and the secondary fluid channel inlet, thereby lowering the liquid level of the reaction liquid in the sample channel.

[0295] In an embodiment of the method, the method includes the following steps:

[0296] - closing the sampling fluid connection and opening the secondary fluid connection,

[0297] - Arrange the multi-way valve to allow fluid flow between the second multi-way connection, the third multi-way connection, and the fourth multi-way connection, or alternatively, arrange the multi-way valve alternately to:

[0298] · Allow fluid flow between the third multi-way connection and the fourth multi-way connection, and arrange to

[0299] · Allow fluid flow between the second multi-way connection and the third multi-way connection,

[0300] In an embodiment of the method, the step of depressurizing the sample extraction device is performed before collecting a sample from the reactor.

[0301] In an embodiment of the method, the method includes the step of arranging a sampling valve in a sampling position.

[0302] In an embodiment of the method, the method includes the step of arranging a secondary fluid valve in a secondary flow position.

[0303] In a twelfth aspect, the present invention provides a method for sampling reaction liquid from a reactor, the method comprising the following steps:

[0304] - Arrange the multi-way valve to allow fluid communication between the first multi-way connection and the fourth multi-way connection,

[0305] - Arrange the sampling valve in a sampling position,

[0306] - Close the secondary fluid connection,

[0307] - Inject a sampling fluid into the reactor volume via a sampling fluid connection, a multi-way valve, and a secondary fluid channel inlet, thereby forcing reaction liquid from the reactor volume into a sample channel and into a sampling space, thereby filling the sampling space with a sampling volume of the reaction liquid, the sampling volume being equal to the chamber volume,

[0308] - Subsequently arrange the sampling valve in a delivery position,

[0309] - Deliver the sampling volume of the reaction liquid from the sampling space through a sample extraction outlet to a suitable destination.

[0310] In an embodiment of the method, during the injection of the sampling fluid into the reactor volume, the volume in the sample channel is sealed relative to the sampling fluid connection and the secondary fluid connection, such that the pressure in the volume of the sample channel is increased by forcing reaction liquid from the reactor volume into the sample channel.

[0311] In an embodiment of the method, the method includes the following steps:

[0312] - Arrange the multi-way valve to allow fluid communication between the first multi-way connection and the fourth multi-way connection.

[0313] - Inject the sampling fluid into the reactor volume via the sampling fluid connection, the multi-way valve, and the secondary fluid channel inlet, thereby forcing the reaction liquid from the reactor volume into the sample channel, through the sampling valve, and into the buffer volume.

[0314] - Adjust the amount and / or pressure of the sampling fluid injected into the reactor volume to control the liquid level of the reaction liquid in the buffer volume.

[0315] In an embodiment of the method, the method includes the following steps:

[0316] - Control the liquid level of the reaction liquid in the buffer volume by adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume, thereby preventing the reaction liquid forced into the sample channel from reaching the multi-way valve.

[0317] In an embodiment of the method, the method includes the following steps:

[0318] - Arrange the secondary fluid valve in the secondary flow position before injecting the sampling fluid into the reactor volume.

[0319] In an embodiment of the method, the method includes the following steps:

[0320] - Arrange the secondary fluid valve in the secondary blocking position after filling the sampling space with the sampling volume of the reaction liquid.

[0321] In an embodiment of the method, the method includes the following steps: before collecting a sample from the reactor:

[0322] - Arrange the multi-way valve to allow fluid flow between the first multi-way connection and the second multi-way connection and between the third multi-way connection and the fourth multi-way connection.

[0323] - Inject the cleaning fluid from the sampling fluid connection into the reactor volume via the sample channel, thereby blowing any reaction liquid out of the sample channel, where optionally, the cleaning fluid is an inert gas such as nitrogen.

[0324] - Remove the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection.

[0325] In a thirteenth aspect, the present invention provides a method for sampling a reaction liquid, the method combining the steps of at least two embodiments in the embodiments of the eleventh or twelfth aspect.

[0326] As shown above, the sample extraction device according to the present invention may include two three-way valves and two crossovers, or a multi-way valve, or another valve system. It will be clear that these may be replaced by any pipe and / or valve system that can provide the required functions and that can be controlled to (e.g., by configurably interconnecting the sample channel and the secondary channel) form the flow paths required to perform the required method steps.

[0327] These and other aspects of the present invention will be readily understood and better appreciated by reference to the following detailed description and when considered in conjunction with the accompanying drawings, in which like reference numerals identify like parts. It will be clear to those skilled in the art that the features of any of the embodiments above may be combined. BRIEF DESCRIPTION OF THE DRAWINGS

[0328] Embodiments of a laboratory system according to the present invention, an extraction device according to the present invention, and a method according to the present invention will be described by way of example only with reference to the accompanying schematic drawings, in which corresponding reference numerals indicate corresponding parts, and in the drawings:

[0329] Figure 1 A schematic diagram of a laboratory system according to the present invention is shown.

[0330] Figure 2 A schematic diagram of a sample extraction device according to the present invention is shown.

[0331] Figure 3 A laboratory system according to the present invention is shown.

[0332] Figure 4A An embodiment of a sample extraction device according to the present invention is shown.

[0333] Figure 4B Shows when performing the cleaning step Figure 4A of the sample extraction device.

[0334] Figure 4C Shows when performing the flushing step Figure 4A of the sample extraction device.

[0335] Figure 4D Shows when performing the pressure equalization step Figure 4A of the sample extraction device.

[0336] Figure 4E Shows where a sample is withdrawn from the reactor volume Figure 4A of the sample extraction device.

[0337] Figure 4F Shows in the sample delivery configuration Figure 4ASample extraction device

[0338] Figure 5A Shows different embodiments of the sample extraction device according to the present invention

[0339] Figure 5B Shows when performing the cleaning step Figure 5A Sample extraction device

[0340] Figure 5C Shows when performing the rinsing step Figure 5A Sample extraction device

[0341] Figure 5D Shows when performing the first part of the pressure equalization step Figure 5A Sample extraction device

[0342] Figure 5E Shows when performing the second part of the pressure equalization step Figure 5A Sample extraction device

[0343] Figure 5F Shows where a sample is withdrawn from the reactor volume Figure 5A Sample extraction device

[0344] Figure 5G Shows in the sample delivery configuration Figure 5A Sample extraction device

[0345] Figure 5H Shows yet another different embodiment of the sample extraction device according to the present invention Detailed implementation

[0346] Figure 1A schematic view of a laboratory system 1 according to the present invention is shown. The laboratory system 1 includes five reactors 2A, 2B, 2C, 2D, 2E, such as thermal cycling reactors, each of the five reactors being associated with a respective sample extraction device 3A, 3B, 3C, 3D, 3E for extracting a sample from the reactors 2A, 2B, 2C, 2D, 2E. The laboratory system 1 further includes a fluid supply system 6, which includes a delivery fluid supply device 10 for supplying a delivery fluid. The delivery fluid includes nitrogen or any other suitable fluid, such as a substantially inert fluid such as a noble gas. The fluid supply system 6 further includes a quench fluid supply device 7, a dilution fluid supply device 8, and a rinse fluid supply device 9. The fluid supply system 6 is connected to the extraction devices 3A, 3B, 3C, 3D, 3E via a fluid supply channel 13, and the fluid from the fluid supply system 6, such as the delivery fluid from the delivery fluid supply device 10, is conveyed to the extraction devices 3A, 3B, 3C, 3D, 3E through the fluid supply channel 13. Five sample storage containers 11A, 11B, 11C, 11D, 11E are provided for storing samples extracted from the reactors 2A, 2B, 2C, 2D, 2E. The storage containers 11A, 11B, 11C, 11D, 11E are connected to the reactors 2A, 2B, 2C, 2D, 2E via sample extraction channels 14A, 14B, 14C, 14D, 14E.

[0347] When a sample is collected from one of the reactors 2A, 2B, 2C, 2D, 2E, the sample is first extracted from the reactors 2A, 2B, 2C, 2D, 2E into sampling spaces 5A, 5B, 5C, 5D, 5E. Then, the fluid supply system 6 uses the delivery fluid from the delivery fluid supply device 10 to push the sample from the sampling spaces 5A, 5B, 5C, 5D, 5E through the sample extraction channels 14A, 14B, 14C, 14D, 14E to the sample storage containers 11A, 11B, 11C, 11D, 11E.

[0348] The laboratory system 1 may further include a plurality of storage containers 11A, 11B, 11C, 11D, 11E associated with each of the reactors 2A, 2B, 2C, 2D, 2E, such that a plurality of samples can be collected from each of the reactors 2A, 2B, 2C, 2D, 2E. A container selection system (not shown) is provided to associate the sample extraction channels 14A, 14B, 14C, 14D, 14E with one of the plurality of sample storage containers 11A, 11B, 11C, 11D, 11E, such that each sample can be stored in a separate sample storage container 11A, 11B, 11C, 11D, 11E.

[0349] Since the laboratory system 1 includes a plurality of reactors 2A, 2B, 2C, 2D, 2E, a reactor selection system is provided to select the reactor from which a sample is to be collected. Two variants of such a reactor selection system are disclosed, namely an upstream reactor selection system 16 as shown in Figure 1 and a downstream reactor selection system (not shown).

[0350] In the illustrated embodiment, each reactor 2A, 2B, 2C, 2D, 2E is associated with a respective sample extraction device 3A, 3B, 3C, 3D, 3E having a respective sampling space 5A, 5B, 5C, 5D, 5E. The sample extraction devices 3A, 3B, 3C, 3D, 3E are configured to extract a sample from the reactors 2A, 2B, 2C, 2D, 2E into the sampling spaces 5A, 5B, 5C, 5D, 5E. Each sample extraction device 3A, 3B, 3C, 3D, 3E is connected to a respective sample storage container 11A, 11B, 11C, 11D, 11E through a sample extraction channel 14A, 14B, 14C, 14D, 14E. A fluid supply channel 13 connects a fluid supply system 6 to each sample extraction device 3A, 3B, 3C, 3D, 3E. An upstream reactor selection system 16 including a 5-way valve 17 arranged in the fluid supply channel 13 is provided to place the selected sample extraction device 3A, 3B, 3C, 3D, 3E of one of the reactors 2A, 2B, 2C, 2D, 2E in fluid communication with the fluid supply system 6. In Figure 1 the sample extraction device 3D of the fourth reactor 2D is shown in fluid communication with the fluid supply system 6, while the sample extraction devices 3A of the first reactor 2A, 3B of the second reactor 2B, 3C of the third reactor 2C, and 3E of the fifth reactor 2E are not in fluid communication with the fluid supply system 6. In an alternative embodiment, each sample extraction device 3A, 3B, 3C, 3D, 3E may include a valve for regulating fluid communication with the fluid supply system 6 such that the 5-way valve 17 is not required.

[0351] Alternatively, a single sample extraction device 3 connected to each of the reactors 2A, 2B, 2C, 2D, 2E via a downstream reactor selection system may be used. In such an embodiment, the downstream reactor selection system determines the reactor 2A, 2B, 2C, 2D, 2E from which the single sample extraction device 3 is to collect a sample. Such a downstream reactor selection system may also include a 5-way valve for placing the sample extraction device 3 in fluid communication with one of the reactors 2A, 2B, 2C, 2D, 2E.

[0352] Figure 2A schematic view of the sample extraction device 3 is shown in more detail. The sample extraction device 3 includes a sample channel 21 extending into the reactor volume 22 of the reactor 2. The sample channel 21 has a sample channel inlet 23, and the sample channel inlet 23 is arranged below the liquid level 24 of the reaction liquid in the reactor volume 22 of the reactor 2. A sampling valve 25 is provided in the sample channel 21, and the sampling valve 25 is movable (e.g., rotatable) between a sampling position 29 and a delivery position 30. The sampling valve 25 is arranged above the liquid level 24 of the reaction liquid. In the sampling position 29, a sampling space 5 having a cavity volume provided in the sampling valve 25 is in fluid communication with the sample channel 21, and in the delivery position 30, the sampling space 5 is in fluid communication with a fluid supply channel 13 and is in fluid communication with a sample extraction channel 14 via a sample extraction outlet 20. The sample extraction device 3 further includes a secondary fluid channel 26 extending into the reactor volume 22, and the secondary fluid channel 26 includes a secondary fluid channel inlet 27 arranged in the reactor volume 22. The secondary fluid channel 26 can be connected to a delivery fluid supply device 10.

[0353] Sampling can be initiated by registering a sample trigger such as time measurement, temperature measurement, measurement of reactor process parameters such as crystallization parameters, transmittance measurement, or any other measurement reaching a certain threshold, or user input, or any other trigger. Collecting a sample using the laboratory system 1 includes first using the reactor selection system 16 to select reactors 2A, 2B, 2C, 2D, 2E. Then, the sample is extracted from the reactors 2A, 2B, 2C, 2D, 2E into the sampling spaces 5A, 5B, 5C, 5D, 5E of the associated sample extraction devices 3A, 3B, 3C, 3D, 3E. Subsequently, the sample is delivered via the sample extraction channels 14A, 14B, 14C, 14D, 14E to the sample storage containers 11A, 11B, 11C, 11D, 11E by supplying a delivery fluid to the sampling spaces 5A, 5B, 5C, 5D, 5E via the fluid supply channel 13. Thus, a sample can be collected under reactor conditions to minimize interference with reactor processes occurring inside the reactor, such as chemical processes and crystallization processes. Return reference Figure 1, the sampling valve 25D of the sample extraction device 3D of the fourth reactor 2D is arranged in the conveying position 30 such that the sampling space 5D is in fluid communication with the fluid supply channel 13 and is in fluid communication with the sample extraction channel 14D via the sample extraction outlet 20D. The sampling valves 25A of the sample extraction device 3A of the first reactor 2A, the sampling valves 25B of the sample extraction device 3B of the second reactor 2B, the sampling valves 25C of the sample extraction device 3C of the third reactor 2C, and the sampling valves 25E of the sample extraction device 3E of the fifth reactor 2E are arranged in the sampling position 29 such that the corresponding sampling spaces 5A, 5B, 5C, 5E are in fluid communication with the fluid supply channel 13 and are in fluid communication with the corresponding sample extraction channels 14A, 14B, 14C, 14E via the corresponding sample extraction outlets 20A, 20B, 20C, 20E.

[0354] As an additional step, a quench fluid for eliminating chemical reactions occurring in the sample can be supplied from the quench fluid supply device 7 to the sample. The quench fluid supply device 7 is preferably connected to the sample extraction devices 3A, 3B, 3C, 3D, 3E via the fluid supply channel 13, preferably connected to the sample extraction devices via the fluid supply channel 13 downstream of the conveying fluid supply device 10. In this way, the conveying fluid can be used to convey the quench fluid to the sampling spaces 5A, 5B, 5C, 5D, 5E. The quench fluid can be supplied to the sample before, during, or after the sample is conveyed to the sample storage containers 11A, 11B, 11C, 11D, 11E. Before the sample is conveyed to the sample storage containers 11A, 11B, 11C, 11D, 11E, the quench fluid may already be present in the sample storage containers 11A, 11B, 11C, 11D, 11E.

[0355] As an additional step, a dilution fluid for diluting the sample can be supplied from the dilution fluid supply device 8 to the sample. The dilution fluid supply device 8 is preferably connected to the sample extraction devices 3A, 3B, 3C, 3D, 3E via the fluid supply channel 13, preferably connected to the sample extraction devices via the fluid supply channel 13 downstream of the conveying fluid supply device 10. In this way, the conveying fluid can be used to convey the dilution fluid to the sample. The dilution fluid can be supplied to the sample before, during, or after the sample is conveyed to the sample storage containers 11A, 11B, 11C, 11D, 11E. Before the sample is conveyed to the sample storage containers 11A, 11B, 11C, 11D, 11E, the dilution fluid may already be present in the sample storage containers 11A, 11B, 11C, 11D, 11E.

[0356] As an additional step, after storing the sample in the sample storage containers 11A, 11B, 11C, 11D, 11E, a flushing fluid can be supplied to the fluid supply channels 13 and the sampling spaces 5A, 5B, 5C, 5D, 5E and the sample extraction channels 14A, 14B, 14C, 14D, 14E. The flushing fluid then deposits in the waste container 19. This ensures that after sampling, no residue remains in the fluid supply channels 13 and the sampling spaces 5A, 5B, 5C, 5D, 5E and the sample extraction channels 14A, 14B, 14C, 14D, 14E, so that the next sample is not contaminated by such residue.

[0357] Using a delivery fluid to deliver a quenching fluid, a dilution fluid, and / or a flushing fluid through at least a portion of the fluid supply channels 13, the sampling spaces 5A, 5B, 5C, 5D, 5E, and / or the sample extraction channels 14A, 14B, 14C, 14D, 14E provides an effective way to deliver these fluids. Additionally, using a delivery fluid to subsequently deliver two fluids can create a separation between the two fluids. This prevents, for example, the quenching liquid and the dilution fluid from mixing in these channels when subsequently being delivered through the fluid supply channels 13, the sampling spaces 5A, 5B, 5C, 5D, 5E, and / or the sample extraction channels 14A, 14B, 14C, 14D, 14E. The use of a delivery fluid for delivering a quenching fluid, a dilution fluid, and / or a flushing fluid can be combined with a fluid pump, such as the fluid pumps provided in the quenching fluid supply device 7, the dilution fluid supply device 8, and the flushing fluid supply device 9.

[0358] When the sampling valve 25 is in the sampling position 29, extracting the sample from the reactor 2 into the sampling space 5 is performed by injecting the delivery fluid via the secondary fluid channel 26 into the reactor volume 22, thereby creating a pressure difference between the reactor volume 22 and the sampling space 5. This forces the fluid in the reactor volume 22 to enter the sample channel 21 via the sample channel inlet 23 and into the sampling space 5. The pressure in the reactor volume 22 and the injection of the delivery fluid into the reactor volume 22 are controlled via the sampling control valves 321, 322, 323, 324. The first sampling control valve 321 and the second sampling control valve 322 are connected to the secondary fluid channel 26 via the secondary fluid valve 31. The third sampling control valve 323 and the fourth sampling control valve 324 are connected to the sample channel 21 via the sampling valve 25.

[0359] After a sample is withdrawn from reactor 2 into the sampling space 5, the sampling valve 25 is arranged in the delivery position 30. Then, a sample volume including the reaction liquid from reactor 2 is present in the sampling space 5, and the sample volume is equal to the chamber volume of the sampling space 5. The sample is then conveyed from the sampling space 5 through the sample extraction outlet 20 into the sample extraction channel and from the sample extraction channel into the sample storage container 11 or any other suitable destination.

[0360] Figure 3 A laboratory system 1 according to the present invention is shown. A plurality of sample storage containers 11 are provided for each of the reactors 2A, 2B, 2C, 2D, 2E such that a plurality of samples can be taken from each of the reactors 2A, 2B, 2C, 2D, 2E.

[0361] In Figures 4A to 5E valves are drawn as double triangles or triple triangles. A solid black triangle indicates that the connection of the valve is closed, while a white-filled triangle indicates that the connection of the valve is open. Thus, a closed inline valve is drawn as two solid black triangles (see, for example, Figure 4A valve 83 in Figure 4B ), and an open inline valve is drawn as two white-filled triangles (see, for example,

[0362] Figures 4A to 4F An embodiment of a sample extraction device 3 according to the present invention is shown. Figures 5A to 5G A different embodiment of a sample extraction device 3 according to the present invention is shown. Figure 5H Yet another embodiment of a sample extraction device 3 according to the present invention is shown. In these three embodiments, the valve system 81 is configured differently. However, in all three embodiments, by appropriate arrangement of the valves of the valve system 81 of these embodiments, the flow paths required to perform the necessary method steps can be formed.

[0363] Figure 4A An embodiment of a sample extraction device 3 according to the present invention is shown. The sample extraction device 3 includes a sample channel 21 extending into the reactor volume 22 of the reactor 2, the sample channel 21 having a sample channel inlet 23 arranged below the liquid level 24 of the reaction liquid in the reactor volume 22 of the reactor 2. The sample extraction device 3 further includes a valve system 81 connected to the sample channel 21, a secondary fluid channel 26, a sampling fluid connection 35, a secondary fluid connection 37, a sample extraction outlet 20, and an exhaust gas connection 80. In Figures 4A to 4FIn the illustrated embodiment, the secondary fluid connection 37 is also the transfer fluid connection 47, the quench fluid connection 89, and the dilution fluid connection 90. Alternatively, the exhaust gas connection 80 can be integrated into the secondary fluid connection 37, while the secondary fluid connection 37 and the transfer fluid connection 47 are separate (see Figures 5A to 5G ). The sampling valve 25 is arranged in the sampling channel 21 and is movable (e.g., rotatable) between a sampling position 29 and a transfer position 30. The sampling valve 25 is arranged above the liquid level 24 of the reaction liquid 33. In the sampling position 29, the sampling space 5 having a chamber volume provided in the sampling valve 25 is in fluid communication with the sample channel 21, and in the transfer position 30, the sampling space 5 is in fluid communication with the transfer fluid connection 47, the quench fluid connection 89, the dilution fluid connection 90, and the sample extraction outlet 20. The sample extraction device 3 further includes a secondary fluid channel 26 extending into the reactor volume 22, and the secondary fluid channel 26 includes a secondary fluid channel inlet 27 arranged in the reactor volume 22, preferably above the liquid level 24 of the reaction liquid 33 in the reactor volume 22.

[0364] The sampling fluid connection 35 is configured to supply pressurized sampling fluid to the sample extraction device 3 via the sampling fluid connection 35, and the sampling fluid is preferably an inert gas such as nitrogen. The sampling valve 25 is arranged between the sampling fluid connection 35 and the sample channel inlet 23. The sampling valve includes a sampling space 5 having a chamber volume and is movable to the sampling position 29 and the transfer position 30. In the sampling position 29, the sampling space is in fluid communication with the sample channel 21. In the transfer position 30, the sampling space is in fluid communication with the sample extraction outlet 20 and the transfer fluid connection 47.

[0365] The secondary fluid valve 31 is arranged in the secondary fluid channel 26, between the secondary fluid connection 37 and the secondary fluid channel inlet 27. The secondary fluid valve 31 is specifically positioned such that there is no additional flow junction between the secondary fluid valve 31 and the secondary fluid channel inlet 27.

[0366] The secondary fluid valve 31 is movable to a secondary blocking position 49, in which the secondary fluid valve 31 blocks the flow through the secondary fluid channel 26. The secondary fluid valve 31 is also movable to a secondary flow position 50, in which the secondary fluid valve 31 allows the flow through the secondary fluid channel 26. When a sample is extracted from the reactor volume 22, the secondary fluid valve 31 is arranged in the secondary flow position 50 before the sampling fluid is injected into the reactor volume 22. After the sampling volume of the sampling space 5 is filled with the reaction liquid 33, the secondary fluid valve 31 is arranged in the secondary blocking position 49.

[0367] The valve system 81 can be arranged in the sampling configuration 82 (seeFigure 4E ) a pressure relief arrangement 86 (see Figure 4D ), a delivery arrangement 87 (see Figure 4F ), and a cleaning arrangement 88 (see Figure 4B ). These arrangements and the method steps performed using these arrangements will now be discussed in more detail.

[0368] In Figure 4B is shown the cleaning arrangement 88 of the valve system 81. The cleaning arrangement 88 is used to clean the sample tube 21 by blowing a cleaning fluid from the cleaning fluid connection 91 through the sample tube 21. In the illustrated embodiment, the cleaning fluid connection 91 is the sampling fluid connection 35 and the cleaning fluid is the sampling fluid. In the cleaning arrangement 88 of the valve system 81, the cleaning fluid connection 91 is in fluid communication with the sample channel inlet 23 and the secondary fluid channel inlet 27 is in fluid communication with the exhaust connection 80. The cleaning fluid is injected from the cleaning fluid connection 91 and the sample channel inlet 23 into the reactor volume. Subsequently, there is a flow from the reactor volume to the secondary fluid channel inlet 27 to the exhaust connection 80. This blows residues and / or reaction liquid out of the sample channel 21 and cleans the sample channel 21.

[0369] As an alternative or addition to cleaning, a flushing step may be performed. Then, the valve system 81 is arranged as shown in Figure 4C . This is a configuration of the valve system 81 similar to the sampling configuration 82 shown in Figure 4E . During the flushing step, the sampling fluid is injected into the reactor volume 22 via the secondary fluid channel inlet 27 such that the liquid level 66 of the reaction liquid 33 in the sample channel 21 is raised. Subsequently, the liquid level of the reaction liquid is lowered by removing fluid from the reactor volume 22 via the secondary fluid channel inlet 27. By repeating this process a number of times, for example two, four or even more times, the sample channel 21 is flushed, but it may also be sufficient to raise and lower the liquid level of the reaction liquid in the sample channel 21 only once. This flushing is preferably performed before a sample is taken. Flushing the sampling tube 21 ensures that any sample taken from the reactor volume 22 includes the reaction liquid 33 from the reactor volume 22 rather than old reaction liquid 33 that may have been left in the sample channel 21 from a previous sampling operation.

[0370] In Figure 4DThe pressure relief configuration 86 of the valve system 81 is shown. The pressure relief configuration 86 is used to depressurize the sample extraction device 3 before collecting a sample. In the pressure relief configuration 86, the sampling valve 25 is in the sampling position 29. And a third flow path 78 and a fourth flow path 79 are formed. The third flow path 77 extends from the secondary fluid channel inlet 27 to the exhaust gas connection 80, and the fourth flow path extends from the sample channel inlet 23 to the exhaust gas connection 80. The secondary fluid channel inlet 27 is in fluid communication with the exhaust gas connection 80 via the third flow path 78, and the sample channel inlet 23 is in fluid communication with the exhaust gas connection 80 via the fourth flow path 79. In this way, both the sample channel 21 and the secondary fluid channel 26 can be depressurized to the pressure of the exhaust gas connection 80 and the exhaust gas region 65 to which the exhaust gas connection 80 is connected. This depressurization is preferably performed before collecting the sample.

[0371] In Figure 4E the sampling configuration 82 of the valve system 81 is shown. The sampling configuration 82 is used when collecting a sample. In the sampling configuration 82, the sampling valve 25 is in the sampling position 29, and the secondary fluid channel inlet 27 is in fluid communication with the sampling fluid connection 35 via the secondary fluid valve 31 in the secondary flow position 50. The sample channel inlet 23 is not in fluid communication with the exhaust gas connection 80. When the valve system 81 is in the sampling configuration 82, the sample blocking valve 83 is arranged in its blocking position 84. This closes the buffer volume 48 from the rest of the system. The buffer volume 48 is arranged between the sampling valve 25 and the sample blocking valve 83, thereby preventing the sample from passing over the sample blocking valve 83 and entering the system. This reduces the risk of damaging or contaminating the system. The sample blocking valve 83 is arranged in the sample channel 21, between the sampling valve 25 and the sampling fluid connection 35 (especially between the sampling valve 25 and the exhaust gas connection 80). Alternatively, the sample blocking valve 83 can be arranged in the sample channel 21, between the sampling valve 25 and the exhaust gas connection 80, for example, if the connections are placed differently such that there is no flow path from the sampling valve 25 to the sampling fluid connection 35.

[0372] To collect a sample, the valve system 81 is arranged in the sampling configuration 82, as Figure 4E shown. The sampling fluid connection 35 is in fluid communication with the secondary fluid channel inlet. This forms a first flow path 76 that extends from the sampling fluid connection 35 to the secondary fluid channel inlet 27. The sampling valve 25 is arranged in the sampling position 29. Then, by injecting the sampling fluid via the first flow path 76 and the secondary fluid channel inlet 27 into the reactor volume 22, the sample is drawn into the sample channel 21 and into the sampling space 5 of the sampling valve 25.

[0373] Thus, the reaction liquid 33 is forced into the sampling space 5 of the sampling valve 25, such that the sampling space 5 is filled with the sampling volume of the reaction liquid 33, and the sampling volume is equal to the chamber volume of the sampling space 5. The liquid level 66 of the reaction liquid 33 in the sample channel 21 rises through the sampling space 5 of the sampling valve 25, and when the sample blocking valve 83 is in its blocking position 84, the pressure in the volume 67 of the sample channel 21 also rises. This sealed volume 67 is the buffer volume 48, which is arranged between the sampling valve 25 and the sampling fluid connection 35. The volume of the buffer volume is selected by choosing the length and width of the tube and / or the volume of the buffer space, such that this rise in pressure is sufficient to provide a suitable reaction force to the reaction liquid rising in the sample channel. The amount and / or pressure of the sampling fluid injected into the reactor is adjusted to control the liquid level of the reaction liquid 33 in the sample channel 21.

[0374] Subsequently, the valve system 81 is arranged in the delivery configuration 87 to form a second flow path 77, see Figure 4F . The delivery configuration 87 is used after the sample has been collected to send the sample to a suitable destination 75. The suitable destination can be, for example, a storage bottle or an analysis tool. In the delivery configuration 87, the sampling valve 25 is in the delivery position 30 configuration, and the secondary fluid connection 37 is in fluid communication with the sampling space 5, such that a second flow path 77 is formed. The second flow path 77 extends from the secondary fluid connection 37 to the sample extraction outlet 20. A delivery fluid, a quenching fluid, and / or a dilution fluid are fed via the second flow path 77 into the sampling space 5.

[0375] In the illustrated embodiment, the secondary fluid connection 37 includes a delivery fluid connection 47, a quenching fluid connection 89, and a dilution fluid connection 90. Thus, in the delivery configuration, the sampling space is also in fluid communication with the delivery fluid connection 47, the quenching fluid connection 89, and the dilution fluid connection 90. In the delivery configuration 87, the sample extraction outlet 20 is in fluid communication with the secondary fluid connection 37 (and the delivery fluid connection 47, the quenching fluid connection 89, and the dilution fluid connection 90), and the sample channel inlet 23 is not in fluid communication with the sampling fluid connection 35.

[0376] Figure 5A An embodiment of a sample extraction device 3 according to the present invention is shown. The sample extraction device 3 includes a sample channel 21 extending into the reactor volume 22 of the reactor 2, the sample channel 21 having a sample channel inlet 23, which is arranged below the liquid level 24 of the reaction liquid in the reactor volume 22 of the reactor 2. The sample extraction device 3 further includes a valve system 81 connected to the sample channel 21, a secondary fluid channel 26, a sampling fluid connection 35, a secondary fluid connection 37, a sample extraction outlet 20, and an exhaust gas connection 80. In Figures 5A to 5HIn the illustrated embodiment, the secondary fluid connection 37 is also the exhaust gas connection 80. A separate delivery fluid connection 47 is also provided. Alternatively, the exhaust gas connection 80 may be separate from the secondary fluid connection 37, while the secondary fluid connection 37 and the delivery fluid connection 47 are integrated (see Figures 4A to 4F ). A sampling valve 25 is provided in the sampling channel 21, and the sampling valve 25 is movable (e.g., rotatable) between a sampling position 29 and a delivery position 30. The sampling valve 25 is arranged above the liquid level 24 of the reaction liquid 33. In the sampling position 29, a sampling space 5 having a chamber volume provided in the sampling valve 25 is in fluid communication with the sample channel 21, and in the delivery position 30, the sampling space 5 is in fluid communication with the delivery fluid connection 47 and the sample extraction outlet 20. The sample extraction device 3 further includes a secondary fluid channel 26 extending into the reactor volume 22, and the secondary fluid channel 26 includes a secondary fluid channel inlet 27 arranged in the reactor volume 22.

[0377] The sampling fluid connection 35 is configured to supply pressurized sampling fluid to the sample extraction device 3 via the sampling fluid connection 35, and the sampling fluid is preferably an inert gas such as nitrogen. The sampling valve 25 is arranged between the sampling fluid connection 35 and the sample channel inlet 23, particularly between the sampling three-way valve 38 and the sample channel inlet 23. The sampling valve includes a sampling space 5 having a chamber volume and is movable to the sampling position 29 and the delivery position 30. In the sampling position 29, the sampling space is in fluid communication with the sample channel 21. In the delivery position 30, the sampling space is in fluid communication with the sample extraction outlet 20 and the delivery fluid connection 47.

[0378] The sample extraction device 3 includes a sampling three-way valve 38 arranged in the sample channel 21 between the sampling fluid connection 35 and the sample channel inlet 23. The sampling three-way valve 38 includes a first sampling connection 39, a second sampling connection 40, and a third sampling connection 41. The first sampling connection 39 and the second sampling connection 40 are connected in series with the sample channel 21, and the third sampling connection 41 is connected to a sampling cross tube 43, and the sampling cross tube 43 is connected to the secondary fluid channel 26 at a secondary cross connection 44. The first sampling connection 39 is arranged between the second sampling connection 40 and the sampling fluid connection 35, and the second sampling connection 40 is arranged between the first sampling connection 39 and the sample channel inlet 23. The sampling cross connection is arranged between the sampling three-way valve 38 and the sampling valve 25.

[0379] The sampling three-way valve 38 is movable to a sampling in-line through position 45, wherein fluid flow between the first sampling connection 39 and the second sampling connection 40 is permitted and wherein fluid flow through the third sampling connection 41 is not permitted. The sampling three-way valve 38 is also movable to a first sampling cross position 46, wherein fluid flow between the first sampling connection 39 and the third sampling connection 41 is permitted and wherein fluid flow through the second sampling connection 40 is not permitted.

[0380] The sample extraction device 3 includes a secondary three-way valve 51 disposed in the secondary fluid passage 26. The secondary three-way valve includes a first secondary connection 52, a second secondary connection 53, and a third secondary connection 54. The first secondary connection 52 and the second secondary connection 53 are connected in-line with the secondary fluid passage 26, and the third secondary connection 54 is connected to a secondary crossover tube 55 that is connected to the sample passage 21 at a sampling crossover connection 56. The first secondary fluid connection 52 is disposed between the second secondary fluid connection 53 and the secondary fluid connection 37. The second secondary fluid connection 53 is disposed between the first secondary fluid connection 51 and the secondary fluid passage inlet 27.

[0381] The sampling three-way valve 38 is disposed between the sampling fluid connection 35 and the sampling fluid passage inlet 23. In particular, the sampling three-way valve 38 is disposed between the sampling fluid connection 35 and the sampling crossover connection 56.

[0382] The secondary three-way valve 51 is disposed between the secondary fluid connection 37 and the secondary fluid passage inlet 27. In particular, the secondary three-way valve 51 is disposed between the secondary fluid connection 37 and the secondary crossover connection 44. The secondary crossover connection 44 is disposed between the secondary three-way valve 51 and the secondary fluid valve 31.

[0383] The secondary three-way valve 51 is movable to a secondary in-line through position 57, wherein fluid flow between the first secondary connection 52 and the second secondary connection 53 is permitted and wherein fluid flow through the third secondary connection 54 is not permitted. The secondary three-way valve 51 is also movable to a first secondary cross position 58, wherein fluid flow between the first secondary connection 52 and the third secondary connection 54 is permitted and wherein fluid flow through the second secondary connection 53 is not permitted.

[0384] The secondary fluid valve 31 is arranged in the secondary fluid passage 26, especially between the secondary fluid connection 37 and the secondary fluid passage inlet 27, in particular between the secondary three-way valve 51 and the secondary fluid passage inlet 27. The secondary fluid valve 31 is movable to a secondary blocking position 49, in which the secondary fluid valve 31 blocks the flow through the secondary fluid passage 26. The secondary fluid valve 31 is also movable to a secondary flow position 50, in which the secondary fluid valve 31 allows the flow through the secondary fluid passage 26. When a sample is taken from the reactor volume 22, the secondary fluid valve 31 is arranged in the secondary flow position 50 before the sampling fluid is injected into the reactor volume 22. After the sampling volume in the sampling space 5 is filled with the reaction liquid 33, the secondary fluid valve 31 is arranged in the secondary blocking position 49.

[0385] The sampling two-way valve 59 is arranged in the sample passage 21, especially between the sampling fluid connection 35 and the sampling valve 25, in particular between the sampling fluid connection 35 and the sampling three-way valve 38. The sampling two-way valve 59 is movable to a sampling open position 60 that allows the flow through the sampling two-way valve 59, and is movable to a sampling closed position 61 that does not allow the flow through the sampling two-way valve 59. The secondary two-way valve 62 is arranged in the secondary fluid passage 26, especially between the secondary fluid connection 37 and the secondary fluid valve 31, in particular between the secondary fluid connection 37 and the secondary three-way valve 51. The secondary two-way valve 62 is movable to a secondary closed position 64, in which the secondary two-way valve 62 blocks the flow through the secondary fluid passage 31, and is movable to a secondary open position 63, in which the secondary two-way valve 62 allows the flow through the secondary fluid passage 26.

[0386] To take a sample, the sampling fluid is injected into the reactor volume 22 via the secondary fluid passage inlet 27 while the volume 67 of the sample passage 21 is sealed relative to the sampling fluid connection 35 and the secondary fluid connection 37, thereby raising the liquid level 66 of the reaction liquid 33 in the sample passage 21 and raising the pressure in the volume 67 of the sample passage 21, and the sample is drawn into the sample passage 21. Then, the sample is taken from the sample passage 21 and moved to a suitable destination 75, such as for storage or further processing. Figure 5F Shown when taking a sample Figure 5AThe sample extraction device 3. The valve system 81 is arranged in the sampling configuration 82 to form a first flow path 76. The sampling fluid connection 35 is in fluid communication with the secondary fluid channel inlet 27 to form a first flow path 76 extending from the sampling fluid connection 35 via the sampling three-way valve 38 to the secondary fluid channel inlet 27. The sampling three-way valve 38 is arranged in the first sampling intersection position 46, the sampling valve 25 is arranged in the sampling position 29, and the secondary fluid connection 37 is closed by arranging the secondary two-way valve 62 in the secondary closed position 64. The sampling fluid is injected into the reactor volume 22 along the first flow path 76 via the sampling fluid connection 35, the sampling three-way valve 38, and the secondary fluid channel inlet 27, thereby raising the liquid level 66 of the reaction liquid 33 in the sample channel 21 above the sampling valve 25. Then, the reaction liquid 33 is forced into the sampling space 5 of the sampling valve 25 such that its sampling volume filled with the reaction liquid 33 is equal to the chamber volume of the sampling space 5. Then, the valve system 81 is arranged in the delivery configuration 87 to form a second flow path 77. The sampling valve is arranged in the delivery position 30, and the secondary fluid valve 31 is arranged in the secondary blocking position 49 (see Figure 5G ). Then, the sampling volume of the reaction liquid 33 is delivered to a suitable destination 75 through the sample extraction outlet by supplying delivery fluid, quench fluid, and / or dilution fluid via the delivery fluid connection 47, the quench fluid connection 89, and / or the dilution fluid connection 90, respectively. In the illustrated embodiment, the delivery fluid connection 47, the quench fluid connection 89, and the dilution fluid connection 90 are integrated into a single connection. During sampling, during the injection of the sampling fluid into the reactor volume 22, the volume 67 of the sample channel 21 is sealed relative to the sampling fluid connection 35 and the secondary fluid connection 37 such that the pressure in the volume 67 of the sample channel 21 is increased by forcing the reaction liquid from the reactor volume 22 into the sample channel 21. This change in pressure is related to the amount of sampling fluid injected into the reactor volume 22 and the liquid level to which the reaction liquid 33 rises in the sample channel 21. The sealing is achieved by arranging the sampling three-way valve 38 in the first sampling intersection position 46 and the secondary three-way valve in the secondary in-line through position while arranging the secondary two-way valve 62 in the secondary closed position 64. Alternatively, a sample blocking valve 83 arranged in the sample channel 21, between the sampling valve 25 and the sampling fluid connection 35 (particularly arranged such that the buffer volume 48 is located between the sampling valve 25 and the sample blocking valve 83) can be used to achieve the sealing. Then, during sampling, the sample blocking valve 83 is arranged in the blocking position 84, and during other operations, the sample blocking valve 83 can be positioned in the blocking position 84 or in the through position 85, depending on whether flow through the sample blocking valve 83 is desired.

[0387] Before collecting a sample, the volumes of the sample channel 21, the secondary fluid channel 26, and the reactor volume 22 can be depressurized by fluidly connecting them to the exhaust gas region 65. Additionally or alternatively, the sample tube 21 can be cleaned by injecting a cleaning fluid from the sampling fluid connection 35 through the sample channel 21 into the reactor volume 22. Any reaction liquid 33 is thereby blown out of the sample channel 21. The cleaning fluid can be an inert gas such as nitrogen. The cleaning fluid is removed from the reactor volume 22 via the secondary fluid channel 26 and the secondary fluid connection 37.

[0388] During Figure 5B the cleaning of the sample tube 21 is shown. The valve system 81 is arranged in the cleaning configuration 88. The sampling three-way valve 38 is arranged in the sampling in-line through position 45. The secondary three-way valve 51 is arranged in the secondary in-line through position 57. A cleaning fluid is injected from the sampling fluid connection 35 through the sample channel 21 into the reactor volume 22, thereby blowing any reaction liquid 33 out of the sample channel 21.

[0389] The sampling valve 5 is arranged above the liquid level 24 of the reaction liquid 33 in the reactor volume 22. A buffer volume 48 is arranged in the sample channel 21, between the sampling valve 5 and the sampling fluid connection 35 (in particular between the sampling valve 5 and the sampling three-way valve 38). When collecting a sample, the amount and / or pressure of the sampling fluid injected into the reactor volume 22 is controlled to control the liquid level 66 of the reaction liquid 33 in the buffer volume 48. This prevents the reaction liquid 33 from reaching the sampling three-way valve 38, thereby reducing the risk of contamination or damage to the sampling three-way valve 38. The volume of the buffer volume 48 is selected such that the reaction liquid 33 completely fills the sampling valve 25 without overshooting, such that it reaches the sampling three-way valve 38 within the range of the reaction liquid density and viscosity in the reactor volume 22 and the volume of the reaction liquid 33.

[0390] Figure 5CIllustrates the flushing step of the sample extraction device 3. The sampling fluid is injected into the reactor volume 22 via the secondary fluid channel inlet 27, thereby raising the liquid level 66 of the reaction liquid 33 in the sample channel 21. Subsequently, the fluid is removed from the reactor volume via the secondary fluid channel inlet 27, thereby lowering the liquid level 66 of the reaction liquid 33 in the sample channel 21. This flushing of the sample tube 21 is repeated multiple times such that any sample collected from the reactor volume 22 comprises the reaction liquid 33 from the reactor volume 22 rather than the old reaction liquid 33 that may remain in the sample channel 21 from a previous sampling operation. To achieve this, the sampling three-way valve 38 is arranged in the first sampling crossover position 46. Then, the sampling fluid is injected into the reactor volume 22 via the sampling fluid connection, the sampling three-way valve 38, and the secondary fluid channel inlet 27 to raise the liquid level 66 of the reaction liquid 33 in the sample channel 21. Subsequently, the fluid is removed from the reactor volume 22 via the sampling fluid connection 35, the sampling three-way valve 38, and the secondary fluid channel inlet 27 to lower the liquid level 66 of the reaction liquid 33 in the sample channel 21.

[0391] Figure 5D and Figure 5E illustrates the sample extraction device 3 when the pressure is equalized Figure 4A of the sample extraction device 3. The sampling valve 25 is arranged in the sampling position 29, and the secondary valve 31 is arranged in the secondary flow position 50. By arranging the sampling two-way valve 59 in the sampling closed position 61 and the secondary two-way valve 62 in the secondary open position 63, the sampling fluid connection 35 is closed and the secondary fluid connection 37 is opened. The sampling three-way valve 38 is arranged in the first sampling crossover position 46. The secondary three-way valve 51 is alternately arranged in the secondary in-line through position 57 (see Figure 4D ) and the first secondary crossover position 58 (see Figure 4E ). This is repeated until the pressure in the reactor volume 22 and the sample channel 21 is sufficiently equalized with the pressure of the secondary fluid connection 37.

[0392] Figure 5H Illustrates an embodiment of the sample extraction device 3 according to the present invention, wherein, compared with Figures 5A to 5F the embodiment shown in Figures 5A to 5FSimilarly to the embodiment shown, the sample extraction device 3 includes a sample channel 21 extending into the reactor volume 22 of the reactor 2, where the sample channel inlet 23 is arranged below the liquid level 24 of the reaction liquid in the reactor volume 22 of the reactor 2. A sampling valve 25 is provided in the sampling channel 21, and the sampling valve 25 is movable (e.g., rotatable) between a sampling position 29 and a delivery position 30. The sampling valve 25 is arranged above the liquid level 24 of the reaction liquid 33. In the sampling position 29, a sampling space 5 having a chamber volume provided in the sampling valve 25 is in fluid communication with the sample channel 21, and in the delivery position 30, the sampling space 5 is in fluid communication with the delivery fluid connection 47 and the sample extraction outlet 20. The sample extraction device 3 further includes a secondary fluid channel 26 extending into the reactor volume 22, and the secondary fluid channel 26 includes a secondary fluid channel inlet 27 arranged in the reactor volume 22.

[0393] The sampling valve 25 is arranged between the sampling fluid connection 35 and the sample channel inlet 23, particularly between the multi-way valve 70 and the sample channel inlet 23. The sampling valve includes a sampling space 5 having a chamber volume and is movable to the sampling position 29 and the delivery position 30. In the sampling position 29, the sampling space is in fluid communication with the sample channel 21. In the delivery position 30, the sampling space is in fluid communication with the sample extraction outlet 20 and the delivery fluid connection 47.

[0394] A secondary fluid valve 31 is arranged in the secondary fluid channel 26 between the secondary fluid connection 37 and the secondary fluid channel inlet 27 (particularly between the multi-way valve 70 and the secondary fluid channel inlet 27). The secondary fluid valve 31 is movable to a secondary blocking position 49, where the secondary fluid valve 31 blocks the flow through the secondary fluid channel 26. The secondary fluid valve 31 is further movable to a secondary flow position 50, where the secondary fluid valve 31 allows the flow through the secondary fluid channel 26. When a sample is extracted from the reactor volume 22, before injecting the sampling fluid into the reactor volume 22, the secondary fluid valve 31 is arranged in the secondary flow position 50. After the sampling volume of the sampling space 5 is filled with the reaction liquid 33, the secondary fluid valve 31 is arranged in the secondary blocking position 49.

[0395] The sampling two-way valve 59 is arranged in the sample channel 21, between the sampling fluid connection 35 and the sampling valve 25, especially between the sampling fluid connection 35 and the multi-way valve 70. The sampling two-way valve 59 can be moved to a sampling open position 60 that allows flow through the sampling two-way valve 59, and can be moved to a sampling closed position 61 that does not allow flow through the sampling two-way valve 59. The secondary two-way valve 62 is arranged in the secondary fluid channel 26, between the secondary fluid connection 37 and the secondary fluid valve 31, especially between the secondary fluid connection 37 and the multi-way valve 70. The secondary two-way valve 62 can be moved to a secondary closed position 64, in which the secondary two-way valve 62 blocks the flow through the secondary fluid channel 31, and can be moved to a secondary open position 63, in which the secondary two-way valve 62 allows the flow through the secondary fluid channel 26.

[0396] The multi-way valve 70 is connected in series with the sample channel 21 via a first multi-way connection 71 and a second multi-way connection 72. The multi-way valve is also connected in series with the secondary fluid channel 26 via a third multi-way connection 73 and a fourth multi-way connection 74. The first multi-way connection 71 is arranged between the second multi-way connection 72 and the sampling fluid connection 35. The second multi-way connection 72 is arranged between the first multi-way connection 71 and the sample channel inlet 23. The third multi-way connection 73 is arranged between the fourth multi-way connection 74 and the secondary fluid connection 37. The fourth multi-way connection 74 is arranged between the third multi-way connection 73 and the secondary fluid channel inlet 27.

[0397] The multi-way valve 70 can be controlled to connect any one of the four multi-way connections 71, 72, 73, 74 to one or more of the other multi-way connections 71, 72, 73, 74. The multi-way valve 70 can, for example, allow flow through the multi-way valve 70 via the first multi-way connection 71 and the second multi-way connection 72 while closing the second multi-way connection 73 and the third multi-way connection 74. Alternatively, flow between the first multi-way connection 71 and the second multi-way connection 72 can be allowed while allowing flow between the third multi-way connection 73 and the fourth multi-way connection 74.

[0398] The multi-way valve 70 can also be controlled to allow flow between other pairs of multi-way connections 71, 72, 73, 74 (e.g., between the first multi-way connection 71 and the fourth multi-way connection 74). This is done, for example, when flushing the sample channel 21. The sampling valve 25 is preferably arranged in the sampling position 29. The secondary fluid valve 31 is arranged in the secondary flow position 50. Then, the sampling fluid is injected into the reactor volume via the sampling fluid connection 35, the multi-way valve 70, and the secondary fluid channel inlet 27, thereby raising the liquid level 66 of the reaction liquid 33 in the sample channel 21. Subsequently, fluid is removed from the reactor volume 22 via the sampling fluid connection 35, the multi-way valve 70, and the secondary fluid channel inlet 27, thereby lowering the liquid level 66 of the reaction liquid 33 in the sample channel 21. This flushes the sample channel 21 with the reaction liquid 33. If desired, the steps of raising and lowering the liquid level 66 of the reaction liquid 33 in the sample channel 21 can be repeated one or more times to ensure that the sample channel 21 is properly flushed. This is comparable to Figure 4C the situation shown in the embodiment including the three-way valves 38, 51 and the cross tubes 43, 55 without including the multi-way valve 70.

[0399] When collecting the sample 4, the multi-way valve 70 is also controlled to allow flow between the first multi-way connection 71 and the fourth multi-way connection 74. The sampling valve 25 is arranged in the sampling position 29. The secondary fluid connection 37 is closed. The secondary fluid valve 31 is arranged in the secondary flow position 50. Then, the sampling fluid is injected into the reactor volume via the sampling fluid connection 35, the multi-way valve 70, and the secondary fluid channel inlet 27, thereby raising the liquid level 66 of the reaction liquid 33 in the sample channel 21 above the sampling valve 25. Then, the reaction liquid 33 is forced into the sampling space 5 of the sampling valve 25 such that the sampling space 5 is filled with a sampling volume of the reaction liquid 33, the sampling volume being equal to the chamber volume of the sampling space 5. Then, the sampling valve is arranged in the delivery position 30, and the secondary fluid valve 31 is arranged in the secondary blocking position 49. Then, the sampling volume of the reaction liquid 33 is delivered to a suitable destination 75 through the sample extraction outlet. During sampling, during the injection of the sampling fluid into the reactor volume 22, the volume 67 of the sample channel 21 is sealed relative to the sampling fluid connection 35 and the secondary fluid connection 37 such that the pressure in the volume 67 of the sample channel 21 is increased by forcing the reaction liquid from the reactor volume 22 into the sample channel 21. This change in pressure is related to the amount of sampling fluid injected into the reactor volume 22 and the liquid level to which the reaction liquid 33 rises in the sample channel 21.

[0400] The sampling valve 5 is arranged above the liquid level 24 of the reaction liquid 33 in the reactor volume 22. The buffer volume 48 is arranged in the sample channel 21, between the sampling valve 5 and the sampling fluid connection 35 (in particular between the sampling valve 5 and the multi-way valve 70). When collecting a sample, the amount and / or pressure of the sampling fluid injected into the reactor volume 22 is controlled to control the liquid level 66 of the reaction liquid 33 in the buffer volume 48. This prevents the reaction liquid 33 from reaching the multi-way valve 70, thereby reducing the risk of contaminating or damaging the multi-way valve 70. The volume of the buffer volume 48 is selected such that the reaction liquid 33 completely fills the sampling valve 25 without overshooting, such that it reaches the multi-way valve 70 within the range of the density and viscosity of the reaction liquid in the reactor volume 22 and the volume of the reaction liquid 33.

[0401] Another use of the multi-way valve is to depressurize the sample extraction device 3 before collecting the sample 4. Here, the sampling fluid connection 35 is closed, for example, by stopping the supply of the sampling fluid or by arranging the sampling two-way valve 59 in the sampling closed position 61. The multi-way valve 70 is controlled to allow fluid flow between the second multi-way connection 72, the third multi-way connection 73 and the fourth multi-way connection 74. This equalizes the pressures in the sample channel 21 and the secondary fluid channel 26. Preferably, the secondary two-way valve 62 is in the secondary open position 63 such that the pressures in the sample channel 21 and the secondary fluid channel 26 are equalized with the pressure in the exhaust gas area 65. The sampling valve 25 is arranged in the sampling position 29 and the secondary fluid valve 31 is arranged in the secondary flow position 50 such that the pressure in the reactor volume 22 is also equalized. This is comparable to Figure 4C the situation shown in the embodiment including the three-way valves 38, 51 and the cross pipes 43, 55 without including the multi-way valve 70. Alternatively, instead of simultaneously allowing fluid flow between the second multi-way connection 72, the third multi-way connection 73 and the fourth multi-way connection 74, the multi-way valve 70 can be controlled to alternately allow fluid flow between the third multi-way connection 73 and the fourth multi-way connection 74 or between the second multi-way connection 72 and the third multi-way connection 73. This is comparable to Figure 5D and Figure 5E the situation shown in the embodiment including the three-way valves 38, 51 and the cross pipes 43, 55 without including the multi-way valve 70.

[0402] Before or after collecting a sample, or at any other suitable moment, the sample tube 21 can be cleaned by blowing a cleaning fluid such as nitrogen through the sample tube 21. The cleaning fluid can be the same fluid as the sample fluid. This can be performed by arranging the multi-way valve 70 to allow fluid flow between the first multi-way connection 71 and the second multi-way connection 72 and between the third multi-way connection 73 and the fourth multi-way connection 74. Then, the cleaning fluid is injected from the sampling fluid connection 35 via the sample channel 21 into the reactor volume 22, thereby blowing any reaction liquid 33 out of the sample channel 21. The cleaning fluid bubbles up through the reaction liquid 33 and is removed from the reactor volume 22 via the secondary fluid channel 26 and the secondary fluid connection 37.

[0403] In Figures 4A to 4F the embodiment shown in, Figures 5A to 5G the embodiment shown in, and in the embodiment shown in 5H, the secondary fluid channel inlet is arranged above the liquid level of the reaction liquid in the reactor.

[0404] Figures 4A to 4F the embodiment shown in, Figures 5A to 5G the embodiment shown in, and the sample extraction device of the embodiment shown in 5H can be incorporated into a cap that can be attached to a reactor vessel in a standard format, and the reactor-cap combination can be "snapped" into a port on the system chassis without an external tube (otherwise it would interfere with human or robotic ergonomics).

[0405] For Figures 4A to 4F the embodiment shown in, Figures 5A to 5G the embodiment shown in, and the different method steps described for the embodiment shown in 5H can be combined to obtain other advantages.

[0406] As needed, detailed embodiments of the present invention are disclosed herein; however, it should be understood that the disclosed embodiments are merely exemplary embodiments of the present invention, and the disclosed embodiments can be implemented in various forms. Therefore, the specific structural and functional details disclosed herein should not be construed as restrictive, but merely as a basis for the claims and as a representative basis for teaching those skilled in the art to employ the present invention in virtually any appropriate detailed structure differently. In addition, the terms and phrases used herein are not intended to be restrictive, but rather to provide an understandable description of the present invention.

[0407] This patent application also relates to the following clauses:

[0408] 1. A sample extraction device configured to extract a sample from a reactor, the sample extraction device comprising:

[0409] - A sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume,

[0410] - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0411] - A sampling fluid connection connected to the sample channel and configured to supply pressurized sampling fluid to the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen,

[0412] - A secondary fluid connection connected to the secondary fluid channel,

[0413] - A sampling three-way valve disposed in the sample channel, the sampling three-way valve including a first sampling connection, a second sampling connection, and a third sampling connection, wherein the first sampling connection and the second sampling connection are connected in series with the sample channel, and wherein the third sampling connection is connected to a sampling cross tube that is connected to the secondary fluid channel at a secondary cross junction, wherein the first sampling connection is disposed between the second sampling connection and the sampling fluid connection, and the second sampling connection is disposed between the first sampling connection and the sample channel inlet,

[0414] Wherein:

[0415] - The sampling three-way valve is disposed between the sampling fluid connection and the sample channel inlet,

[0416] - The sampling three-way valve is movable to a sampling in-line through position, wherein fluid flow between the first sampling connection and the second sampling connection is allowed, and wherein fluid flow through the third sampling connection is not allowed,

[0417] - The sampling three-way valve is movable to a first sampling cross position, wherein fluid flow between the first sampling connection and the third sampling connection is allowed, and wherein fluid flow through the second sampling connection is not allowed.

[0418] 2. The sample extraction device according to clause 1, comprising:

[0419] - A sampling valve disposed in the sample channel,

[0420] - A sample extraction outlet,

[0421] Wherein:

[0422] - The sampling valve is arranged between the sampling fluid connection and the inlet of the sample channel, wherein the sampling valve is preferably arranged between the sampling three-way valve and the inlet of the sample channel.

[0423] - The sampling valve includes a sampling space having a chamber volume.

[0424] - The sampling valve is movable to a sampling position and is movable to a delivery position.

[0425] - In the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel.

[0426] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

[0427] 3. The sample extraction device according to the preceding clause, comprising:

[0428] - A delivery fluid connection for providing a delivery fluid, wherein optionally the delivery fluid is an inert gas, preferably nitrogen.

[0429] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the delivery fluid connection at the delivery position of the sampling valve.

[0430] 4. The sample extraction device according to clause 2 or 3, wherein the sampling valve is configured to be arranged above the liquid level of the reaction liquid in the reactor volume.

[0431] 5. The sampling extraction device according to any one of clauses 2 to 4, wherein the sample channel includes a buffer volume arranged between the sampling valve and the sampling fluid connection, wherein the buffer volume is preferably arranged between the sampling valve and the sampling three-way valve.

[0432] 6. The sample extraction device according to any one of the preceding clauses, comprising:

[0433] - A secondary fluid valve arranged in the secondary fluid channel and between the secondary fluid connection and the inlet of the secondary fluid channel, wherein the secondary fluid valve is preferably arranged between the secondary cross-connection and the inlet of the secondary fluid channel.

[0434] Wherein:

[0435] - The secondary fluid valve is movable to a secondary blocking position, wherein the secondary fluid valve blocks the flow through the secondary fluid channel, and the secondary fluid valve is movable to a secondary flow position, wherein the secondary fluid valve allows the flow through the secondary fluid channel.

[0436] 7. The sample extraction device according to any one of the preceding clauses, comprising:

[0437] - A secondary three-way valve disposed in the secondary fluid passage, the secondary three-way valve including a first secondary connection, a second secondary connection, and a third secondary connection, wherein the first secondary connection and the second secondary connection are connected in series with the secondary fluid passage, and wherein the third secondary connection is connected to a secondary crossover tube that is connected to the sample passage at a sampling crossover junction, wherein the first secondary fluid connection is disposed between the second secondary fluid connection and the secondary fluid connection, and the second secondary fluid connection is disposed between the first secondary fluid connection and the secondary fluid passage inlet,

[0438] Wherein:

[0439] - The secondary three-way valve is disposed between the secondary fluid connection and the secondary fluid passage inlet, wherein the secondary three-way valve is preferably disposed between the secondary fluid connection and the secondary crossover connection,

[0440] - The secondary three-way valve is movable to a secondary in-line through position, wherein fluid flow between the first secondary connection and the second secondary connection is allowed, and wherein fluid flow through the third secondary connection is not allowed,

[0441] - The secondary three-way valve is movable to a first secondary crossover position, wherein fluid flow between the first secondary connection and the third secondary connection is allowed, and wherein fluid flow through the second secondary connection is not allowed.

[0442] 8. The sample extraction device according to the foregoing clause, further comprising the features of clause 8, wherein:

[0443] - The secondary crossover connection is disposed between the secondary three-way valve and the secondary fluid valve.

[0444] 9. The sample extraction device according to clause 7 or 8, the sample extraction device further comprising the features of clause 2, wherein:

[0445] - The sampling crossover connection is disposed between the sampling three-way valve and the sampling valve.

[0446] 10. The sample extraction device according to any one of the foregoing clauses, the sample extraction device further comprising:

[0447] - A sampling two-way valve disposed in the sample passage, between the sampling fluid connection and the sampling three-way valve, wherein the sampling two-way valve is movable to a sampling open position allowing flow through the sampling two-way valve and a sampling closed position not allowing flow through the sampling two-way valve, and / or

[0448] - According to the features of clause 8 and a secondary two-way valve disposed in the secondary fluid passage, between the secondary fluid connection and the secondary three-way valve, wherein the secondary two-way valve is movable to a secondary open position allowing flow through the secondary two-way valve and a secondary closed position not allowing flow through the secondary two-way valve.

[0449] 11. A method of sampling a reaction liquid from a reactor using a sample extraction device, the sample extraction device comprising:

[0450] - A sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume,

[0451] - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0452] - A sampling fluid connection connected to the sample channel, the sampling fluid connection being configured to supply pressurized sampling fluid to the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen,

[0453] - A secondary fluid connection connected to the secondary fluid channel,

[0454] wherein the method comprises the following steps:

[0455] - Depressurizing the volume in the sample channel, the volume in the secondary fluid channel, and the reactor volume by bringing the sample channel and the secondary fluid channel into fluid communication with an exhaust gas region such as the atmosphere,

[0456] - Injecting the sampling fluid into the reactor via the secondary fluid channel inlet while sealing the volume of the sample channel relative to the sampling fluid connection and the secondary fluid connection, thereby raising the liquid level of the reaction liquid in the sample channel and raising the pressure in the volume of the sample channel, and drawing the sample into the sample channel,

[0457] - Extracting the sample from the sample channel and moving it to a suitable destination.

[0458] 12. The method according to the preceding clause, wherein the method comprises the following steps:

[0459] - Injecting a cleaning fluid from the sampling fluid connection into the reactor volume via the sample channel, thereby blowing any reaction liquid out of the sample channel, wherein optionally the cleaning fluid is an inert gas such as nitrogen,

[0460] - Removing the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection, wherein said step is preferably performed before depressurizing and drawing the sample.

[0461] 13. The method according to any one of the preceding method clauses, wherein the method comprises the following steps:

[0462] - Inject the sampling fluid into the reactor volume via the secondary fluid channel inlet, thereby raising the liquid level of the reaction liquid in the sample channel.

[0463] - Subsequently, remove the fluid from the reactor volume via the secondary fluid channel inlet, thereby lowering the liquid level of the reaction liquid in the sample channel.

[0464] Wherein, the steps are preferably performed before decompressing and sampling the sample.

[0465] 14. A method for flushing a sample extraction device according to any one of the preceding device clauses, the method comprising the following steps:

[0466] - Arrange the sampling three-way valve in the first sampling crossover position.

[0467] - Inject the sampling fluid into the reactor volume via the sampling fluid connection, the sampling three-way valve, and the secondary fluid channel inlet, thereby raising the liquid level of the reaction liquid in the sample channel.

[0468] - Subsequently, remove the fluid from the reactor volume via the sampling fluid connection, the sampling three-way valve, and the secondary fluid channel inlet, thereby lowering the liquid level of the reaction liquid in the sample channel.

[0469] 15. A method for decompressing a sample extraction device according to clause 8 or 9, the method comprising the following steps:

[0470] - Close the sampling fluid connection and open the secondary fluid connection.

[0471] - Arrange the sampling three-way valve in the first sampling crossover position.

[0472] - Arrange the secondary three-way valve alternately in the secondary in-line through position and the first secondary crossover position multiple times to equalize the pressures in both the reactor volume and the sample channel with the pressure of the secondary fluid connection.

[0473] 16. A method according to the preceding clauses, wherein the step of decompressing the sample extraction device is performed before sampling the sample from the reactor.

[0474] 17. A method according to clause 15 or 16, wherein the sample extraction device includes the features of clause 2, and the method includes the step of arranging the sampling valve in the sampling position.

[0475] 18. A method according to any one of clauses 15 to 17, wherein the sample extraction device includes the features of clause 7, and the method includes the step of arranging the secondary fluid valve in the secondary flow position.

[0476] 19. A method for sampling reaction liquid from a reactor using a sample extraction device according to any one of clauses 2 to 4, the method comprising the following steps:

[0477] - Arranging a sampling three-way valve in a first sampling intersection position,

[0478] - Arranging a sampling valve in a sampling position,

[0479] - Closing the secondary fluid connection,

[0480] - Injecting a sampling fluid into the reactor volume via a sampling fluid connection, a sampling three-way valve, and a secondary fluid channel inlet, thereby forcing the reaction fluid from the reactor volume into the sample channel and into the sampling space, thereby filling the sampling space with a sampling volume of the reaction liquid, the sampling volume being equal to the cavity volume,

[0481] - Subsequently arranging the sampling valve in a delivery position,

[0482] - Delivering the sampling volume of the reaction liquid from the sampling space to a suitable destination through a sample extraction outlet.

[0483] 20. The method for sampling reaction liquid from a reactor according to the preceding clause, wherein during the injection of the sampling fluid into the reactor volume, the volume in the sample channel is sealed relative to the sampling fluid connection and the secondary fluid connection, such that the pressure in the volume of the sample channel is increased by forcing the reaction fluid from the reactor volume into the sample channel.

[0484] 21. A method for sampling reaction liquid from a reactor using a sample extraction device according to clause 6, the method comprising the following steps:

[0485] - Arranging a sampling three-way valve in a first sampling intersection position,

[0486] - Injecting a sampling fluid into the reactor volume via a sampling fluid connection, a sampling three-way valve, and a secondary fluid channel inlet, thereby forcing the reaction fluid from the reactor volume into the sample channel, through and past the sampling valve, and into a buffer volume,

[0487] - Adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume to control the liquid level of the reaction fluid in the buffer volume.

[0488] 22. The method for sampling reaction liquid according to the preceding clause, the method comprising the following steps:

[0489] - Controlling the liquid level of the reaction fluid in the buffer volume by adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume, thereby preventing the reaction fluid forced into the sample channel from reaching the sampling three-way valve.

[0490] 23. A method for sampling reaction liquid from a reactor using a sample extraction device including the features of clause 7, the method comprising performing the following steps:

[0491] - Before injecting the sampling fluid into the reactor volume, arranging a secondary fluid valve in a secondary flow position.

[0492] 24. The method for sampling reaction liquid from a reactor according to the foregoing clause, the method further including the features of clause 16, the method comprising the following steps:

[0493] - After filling the sampling space with the sampling volume of the reaction liquid, arranging the secondary fluid valve in a secondary blocking position.

[0494] 25. A method for sampling reaction liquid from a reactor using a sample extraction device according to any one of the foregoing device clauses, the method comprising the following steps: Before collecting a sample from the reactor:

[0495] - Arranging a sampling three-way valve in a sampling in-line through position,

[0496] - Arranging a secondary three-way valve in a secondary in-line through position,

[0497] - Injecting a cleaning fluid from the sampling fluid connection via the sample channel into the reactor volume, thereby blowing any reaction liquid out of the sample channel, wherein, optionally, the cleaning fluid is an inert gas such as nitrogen,

[0498] - Removing the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection.

[0499] 26. A method for sampling reaction liquid, the method combining the steps of at least two of the foregoing method clauses.

[0500] 27. A sample extraction device configured to extract a sample from a reactor, the sample extraction device comprising:

[0501] - A sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be arranged below the liquid level of the reaction liquid in the reactor volume,

[0502] - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume,

[0503] - A sampling fluid connection connected to the sample channel, the sampling fluid connection being configured to supply pressurized sampling fluid to the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen.

[0504] - A secondary fluid connection, the secondary fluid connection being connected to the secondary fluid channel.

[0505] - A multi-way valve, wherein the multi-way valve is connected in series with the sample channel via a first multi-way connection and a second multi-way connection, and the multi-way valve is connected in series with the secondary fluid channel via a third multi-way connection and a fourth multi-way connection.

[0506] Wherein:

[0507] - The first multi-way connection is arranged between the second multi-way connection and the sampling fluid connection, the second multi-way connection is arranged between the first multi-way connection and the sample channel inlet, the third multi-way connection is arranged between the fourth multi-way connection and the secondary fluid connection, and the fourth multi-way connection is arranged between the third multi-way connection and the secondary fluid channel inlet.

[0508] - The multi-way valve can be configured to connect any one of the four multi-way connections to one or more of the other multi-way connections.

[0509] 28. The sample extraction device according to the foregoing clause, comprising:

[0510] - A sampling valve arranged in the sample channel.

[0511] - A sample extraction outlet.

[0512] Wherein:

[0513] - The sampling valve is arranged between the sampling fluid connection and the sample channel inlet, and preferably, the sampling valve is arranged between the multi-way valve and the sample channel inlet.

[0514] - The sampling valve includes a sampling space having a cavity volume.

[0515] - The sampling valve can be moved to a sampling position and a delivery position.

[0516] - In the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel.

[0517] - In the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

[0518] 29. The sample extraction device according to the foregoing clause, comprising:

[0519] - A delivery fluid connection for providing a delivery fluid, wherein optionally, the delivery fluid is an inert gas, preferably nitrogen.

[0520] - At the delivery position of the sampling valve, the sampling space is in fluid communication with the delivery fluid at the delivery position of the sampling valve.

[0521] 30. The sample extraction device according to clause 28 or 29, wherein the sampling valve is configured to be arranged above the liquid level of the reaction liquid in the reactor volume.

[0522] 31. The sampling extraction device according to any one of clauses 28 to 30, wherein the sample channel includes a buffer volume arranged between the sampling valve and the sampling fluid connection, and the buffer volume is preferably arranged between the sampling valve and the multi-way valve.

[0523] 32. The sample extraction device according to any one of clauses 27 to 31, comprising:

[0524] - A secondary fluid valve arranged in the secondary fluid channel and between the secondary fluid connection and the secondary fluid channel inlet, and the secondary fluid valve is preferably arranged between the multi-way valve and the secondary fluid channel inlet,

[0525] wherein:

[0526] - The secondary fluid valve can be moved to a secondary blocking position, where the secondary fluid valve blocks the flow through the secondary fluid channel, and the secondary fluid valve can be moved to a secondary flow position, where the secondary fluid valve allows the flow through the secondary fluid channel.

[0527] 33. The sample extraction device according to any one of clauses 27 to 32, the sample extraction device further comprising:

[0528] - A sampling two-way valve arranged in the sample channel, between the sampling fluid connection and the sampling valve, and the sampling two-way valve can be moved to a sampling open position allowing flow through the sampling two-way valve and a sampling closed position not allowing flow through the sampling two-way valve, and / or

[0529] - A secondary two-way valve arranged in the secondary fluid channel, between the secondary fluid connection and the secondary fluid valve, and the secondary two-way valve can be moved to a secondary open position allowing flow through the secondary two-way valve and a secondary closed position not allowing flow through the secondary two-way valve.

[0530] 34. A method of flushing the sample extraction device according to any one of clauses 27 to 33, the method comprising the following steps:

[0531] - Arranging the multi-way valve to allow fluid flow between the first multi-way connection and the fourth multi-way connection and blocking fluid flow through the second multi-way connection,

[0532] - Inject the sampling fluid into the reactor volume via the sampling fluid connection, multi-way valve, and secondary fluid channel inlet, thereby raising the liquid level of the reaction liquid in the sample channel.

[0533] - Subsequently remove fluid from the reactor volume via the sampling fluid connection, multi-way valve, and secondary fluid channel inlet, thereby lowering the liquid level of the reaction liquid in the sample channel.

[0534] 35. A method for depressurizing a sample extraction device according to any one of clauses 27 to 33, the method comprising the steps of:

[0535] - Close the sampling fluid connection and open the secondary fluid connection.

[0536] - Arrange the multi-way valve to allow fluid flow between the second multi-way connection, the third multi-way connection, and the fourth multi-way connection, or alternatively, arrange the multi-way valve alternately to:

[0537] · Allow fluid flow between the third multi-way connection and the fourth multi-way connection and arrange to

[0538] · Allow fluid flow between the second multi-way connection and the third multi-way connection.

[0539] 36. The method according to the preceding clause, wherein the step of depressurizing the sample extraction device is performed before sampling the sample from the reactor.

[0540] 37. The method according to clause 35 or 36, the sample extraction device comprising the features of clause 28, the method comprising the step of arranging the sampling valve in the sampling position.

[0541] 38. The method according to any one of clauses 35 to 37, the sample extraction device comprising the features of clause 32, the method comprising the step of arranging the secondary fluid valve in the secondary flow position.

[0542] 39. A method for sampling reaction liquid from a reactor using a sample extraction device according to clause 28 or 29, the method comprising the following steps:

[0543] - Arrange the multi-way valve to allow fluid communication between the first multi-way connection and the fourth multi-way connection.

[0544] - Arrange the sampling valve in the sampling position.

[0545] - Close the secondary fluid connection.

[0546] - Inject a sampling fluid into the reactor volume via a sampling fluid connection, a multi-way valve, and a secondary fluid channel inlet, thereby forcing reaction fluid from the reactor volume into the sample channel and into the sampling space, thereby filling the sampling space with a sampling volume of the reaction liquid, the sampling volume being equal to the chamber volume.

[0547] - Subsequently arrange the sampling valve in the delivery position.

[0548] - Deliver the sampling volume of the reaction liquid from the sampling space through the sample extraction outlet to a suitable destination.

[0549] 40. A method for sampling reaction liquid from a reactor according to the preceding clause, wherein during injection of the sampling fluid into the reactor volume, the volume in the sample channel is sealed relative to the sampling fluid connection and the secondary fluid connection, such that the pressure in the volume of the sample channel is increased by forcing reaction fluid from the reactor volume into the sample channel.

[0550] 41. A method for sampling reaction liquid from a reactor using a sample extraction device according to clause 31, the method comprising the steps of:

[0551] - Arrange the multi-way valve to allow fluid communication between the first multi-way connection and the fourth multi-way connection.

[0552] - Inject a sampling fluid into the reactor volume via a sampling fluid connection, a multi-way valve, and a secondary fluid channel inlet, thereby forcing reaction fluid from the reactor volume into the sample channel, into and through the sampling valve, and into the buffer volume.

[0553] - Adjust the amount and / or pressure of the sampling fluid injected into the reactor volume to control the level of the reaction fluid in the buffer volume.

[0554] 42. A method for sampling reaction liquid according to the preceding clause, the method comprising the steps of:

[0555] - Control the level of the reaction fluid in the buffer volume by adjusting the amount and / or pressure of the sampling fluid injected into the reactor volume, thereby preventing the reaction fluid forced into the sample channel from reaching the multi-way valve.

[0556] 43. A method for sampling reaction liquid from a reactor using a sample extraction device comprising the features of clause 32, the method comprising performing the steps of:

[0557] - Before injecting the sampling fluid into the reactor volume, arrange the secondary fluid valve in the secondary flow position.

[0558] 44. A method for sampling reaction liquid from a reactor according to the foregoing clauses, the method further comprising the features of clause 36, the method comprising the following steps:

[0559] - After filling the sampling space with the sampling volume of the reaction liquid, arranging the secondary fluid valve in the secondary blocking position.

[0560] 45. A method for reaction liquid from a reactor using a sample extraction device according to any one of clauses 27 to 33, the method comprising the following steps: Before collecting a sample from the reactor:

[0561] - Arranging the multi-way valve to allow fluid flow between the first multi-way connection and the second multi-way connection and fluid flow between the third multi-way connection and the fourth multi-way connection,

[0562] - Injecting a cleaning fluid from the sampling fluid connection via the sample channel into the reactor volume, thereby blowing out any reaction liquid from the sample channel, wherein, optionally, the cleaning fluid is an inert gas such as nitrogen,

[0563] - Removing the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection.

[0564] 46. A method for sampling reaction liquid, the method combining the steps of at least two of method clauses 28 to 45.

[0565] As used herein, the term "a" or "an" is defined as one or more than one. As used herein, the term "plural" is defined as two or more than two. As used herein, the term "another" is defined as at least a second or at least a further one. As used herein, the terms "comprising" and / or "having" are defined as including (i.e., open-ended terms, excluding no other elements or steps). Any reference signs in the claims shall not be construed as limiting the scope of the claims or the invention.

[0566] As used herein, the term "liquid" includes any type of mixture that exhibits liquid-like properties, such as slurries, gels, solid-liquid mixtures, etc.

[0567] The mere fact that certain measures are recited in mutually different dependent claims or clauses does not mean that a combination of these measures cannot be used to advantage.

Claims

1. A method for sampling a reaction liquid from a reactor, wherein, The method comprises the following steps: - providing a sample extraction device comprising the features according to any one of claims 11 to 23, - fluidly connecting the sampling fluid connection with the secondary fluid channel inlet to form a first flow path extending from the sampling fluid connection to the secondary fluid channel inlet, and injecting the sampling fluid into the reactor via the first flow path and the secondary fluid channel inlet while sealing the buffer volume of the sample channel relative to the secondary fluid connection and the exhaust gas connection, thereby raising the liquid level of the reaction liquid in the sample channel and raising the pressure in the buffer volume of the sample channel to draw the sample into the sample channel, - fluidly connecting the secondary fluid connection with the sample extraction outlet to form a second flow path extending from the secondary fluid connection to the sample extraction outlet, and subsequently feeding the secondary fluid to the secondary fluid connection, thereby extracting the sample from the sample channel and moving the sample to a suitable destination.

2. The method according to the preceding claim, wherein, The method comprises the following steps: - depressurizing the volume in the sample channel, the volume in the secondary fluid channel and the reactor volume by arranging the valve system to fluidly connect the sample channel and the secondary fluid channel with the exhaust gas connection, thereby forming a third flow path extending from the secondary fluid channel inlet to the exhaust gas connection and a fourth flow path extending from the sample channel inlet to the exhaust gas connection.

3. The method according to the preceding claim, the sample extraction device comprising the features according to claim 15, wherein, The depressurizing step comprises arranging the valve system in a depressurizing configuration.

4. The method according to any one of the preceding claims, wherein, The method comprises the step of cleaning the sample extraction device by: - injecting a cleaning fluid from the sampling fluid connection into the reactor volume via the sample channel, thereby blowing any reaction liquid out of the sample channel, wherein, optionally, the cleaning fluid is an inert gas such as nitrogen, - removing the cleaning fluid from the reactor volume via the secondary fluid channel and the secondary fluid connection, wherein the step of cleaning the sample extraction device is preferably performed before sampling.

5. The method according to the preceding claim, the sample extraction device comprising the features according to claim 19, wherein, The step of cleaning the sample extraction device comprises arranging the valve system in a cleaning configuration.

6. The method according to any one of the preceding method claims, wherein, The method comprises flushing the sampling tube by performing the following steps: - injecting the sampling fluid into the reactor volume via the secondary fluid channel inlet, thereby raising the liquid level of the reaction liquid in the sample channel, - subsequently removing the fluid from the reactor volume via the secondary fluid channel inlet, thereby lowering the liquid level of the reaction liquid in the sample channel, - optionally repeating the steps of injecting and removing the sampling fluid via the secondary fluid channel inlet, wherein the steps are preferably performed before depressurizing the sample and sampling.

7. The method according to any one of the preceding claims, the sample extraction device comprising the features according to any one of claims 12 to 14, wherein, The step of sampling the sample comprises arranging the valve system in a sampling configuration.

8. The method according to any one of the preceding claims, wherein, The step of sampling the sample comprises the following steps: - Inject the sampling fluid into the reactor volume via the sampling fluid connection, the valve system, and the secondary fluid channel inlet, thereby forcing the reaction liquid from the reactor volume into the sample channel, through the sampling valve, and into the buffer volume of the sample channel. - Adjust the amount and / or pressure of the sampling fluid injected into the reactor volume to control the liquid level of the reaction liquid in the buffer volume.

9. The method according to any one of the preceding claims, the sample extraction device comprising the features according to any one of claims 16 to 18, wherein, The step of extracting the sample and moving the sample to a suitable location includes arranging the valve system in a delivery configuration.

10. The method according to any one of the preceding claims, wherein, The secondary fluid includes a quench fluid and / or a dilution fluid and / or a delivery fluid, and the delivery fluid is preferably an inert gas such as nitrogen.

11. A sample extraction device configured to extract a sample from a reactor, the sample extraction device comprising: - A sample channel configured to extend into the reactor volume of the reactor, the sample channel including a sample channel inlet configured to be disposed below the liquid level of the reaction liquid in the reactor volume. - A secondary fluid channel configured to extend into the reactor volume, the secondary fluid channel including a secondary fluid channel inlet configured to be in fluid communication with the reactor volume. - A sampling fluid connection connected to the sample channel, the sampling fluid connection being configured to provide pressurized sampling fluid to a sample extraction device via the sampling fluid connection, wherein the sampling fluid is preferably an inert gas such as nitrogen. - A secondary fluid connection - A sample extraction outlet - An exhaust gas connection - A buffer volume disposed between the sampling valve and the sampling fluid connection. - A valve system connected to the sample channel, the secondary fluid channel, the sampling fluid connection, the secondary fluid connection, the sample extraction outlet, and the exhaust gas connection. The valve system includes a sampling valve. Wherein: - The sampling valve is disposed between the sampling fluid connection and the sample channel inlet. - The sampling valve includes a sampling space having a chamber volume. - The sampling valve is movable to a sampling position and movable to a delivery position. - In the sampling position of the sampling valve, the sampling space is in fluid communication with the sample channel. - In the delivery position of the sampling valve, the sampling space is in fluid communication with the sample extraction outlet.

12. The sample extraction device according to any one of the preceding device claims, wherein, The valve system can be arranged in a sampling configuration, wherein in the sampling configuration: - The sampling valve is in the sampling position. - The secondary fluid channel inlet is in fluid communication with the sampling fluid connection. - The sample channel inlet is not in fluid communication with the exhaust gas connection.

13. The sample extraction device according to the preceding claims, wherein, The valve system includes a sample blocking valve disposed in the sample channel between the sampling valve and the sampling fluid connection, wherein the sample blocking valve is disposed in a blocking position in the sampling configuration of the valve system.

14. The sample extraction device according to the preceding claims, wherein, The buffer volume is disposed between the sampling valve and the sample blocking valve.

15. The sample extraction device according to any one of the preceding device claims, wherein, The valve system can be arranged in a decompression configuration, wherein in the decompression configuration: - The sampling valve is in the sampling position. - The inlet of the secondary fluid passage is in fluid communication with the exhaust gas. - The inlet of the sample passage is in fluid communication with the exhaust gas.

16. The sample extraction device according to any one of the preceding device claims, wherein, The valve system can be arranged in a delivery configuration, in which: - The sampling valve is in the delivery position. - The secondary fluid connection is in fluid communication with the sampling space.

17. The sample extraction device according to the preceding claims, wherein, In the delivery configuration: - The sample extraction outlet is in fluid communication with the secondary fluid connection, and / or - The inlet of the sample passage is not in fluid communication with the sampling fluid connection.

18. The sample extraction device according to claim 16 or 17, wherein: - The secondary fluid connection includes a delivery fluid connection for providing a delivery fluid, wherein optionally, the delivery fluid is an inert gas, preferably nitrogen. - In the delivery position of the sampling valve, the sampling space is in fluid communication with the delivery fluid connection.

19. The sample extraction device according to any one of the preceding device claims, wherein the sample extraction device includes a cleaning fluid connection, wherein, The valve system can be arranged in a cleaning configuration, wherein optionally, the cleaning fluid connection is the sampling fluid connection, and in the cleaning configuration: - The cleaning fluid connection is in fluid communication with the inlet of the sample passage. - The inlet of the secondary fluid passage is in fluid communication with the exhaust gas.

20. The sample extraction device according to any one of the preceding device claims, wherein: - The secondary fluid connection includes a quench fluid connection for providing a quench fluid. - In the delivery position of the sampling valve, the sampling space is in fluid communication with the quench fluid connection.

21. The sample extraction device according to any one of the preceding device claims, wherein: - The secondary fluid connection includes a dilution fluid connection for providing a dilution fluid. - In the delivery position of the sampling valve, the sampling space is in fluid communication with the dilution fluid connection.

22. The sample extraction device according to any one of the preceding device claims, wherein, The sampling valve is configured to be arranged above the liquid level of the reaction liquid in the reactor volume.

23. The sample extraction device according to any one of the preceding device claims, wherein, The valve system includes: - A secondary fluid valve arranged in the secondary fluid passage and between the secondary fluid connection and the inlet of the secondary fluid passage. Wherein: - The secondary fluid valve can be moved to a secondary blocking position, in which the secondary fluid valve blocks the flow through the secondary fluid passage, so that the flow through the inlet of the secondary fluid passage is blocked, and the secondary fluid valve can be moved to a secondary flow position, in which the secondary fluid valve allows the flow through the secondary fluid passage and allows the flow through the inlet of the secondary fluid passage.

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