Monitoring device for the monitoring of chemical reactions by means of MR measurements in a flow cell

Patent metadata

Field	Value
Publication number	US-10816489-B2
Application number	US-201715812708-A
Country	US
Kind code	B2
Filing date	Nov 14, 2017
Priority date	Nov 15, 2016
Publication date	Oct 27, 2020
Grant date	Oct 27, 2020

Abstract

A monitoring device is provided for analytical measurement of reaction fluid produced in a reaction vessel in a spectrometer with a monitoring cell. The distribution apparatus includes at least four supply and return lines that open into the distribution apparatus, wherein the distribution apparatus comprises a distribution device for distributing reaction fluid to the supply and return lines. The distribution apparatus comprises a distribution vessel in which the distribution device and an electrically controllable pump device for pumping of the reaction fluid are provided, wherein the distribution device comprises an electrically controllable valve device for distributing the reaction fluid to the lines that open into the distribution vessel. A control and regulating device for electrical control of the pump device and of the valve device is provided, wherein reaction control is prompt, automated, and optimized with respect to process parameters, and wherein temperature control may include the entire flow path.

First claim

What is claimed is:

1. A monitoring device for conducting an analytical measurement of a reaction fluid comprising:
a reaction vessel containing the reaction fluid;
a spectrometer for measuring the reaction fluid;
a monitoring cell arranged in the spectrometer for receiving the reaction fluid to be measured in the spectrometer and transporting the reaction fluid back to the reaction vessel;
a distribution apparatus for distributing the reaction fluid between the monitoring cell and the reaction vessel, comprising a distribution device, coupled to a first supply line and a first return line for supplying the reaction fluid from the reaction vessel to the distribution device and for returning the reaction fluid from the distribution device to the reaction vessel, and coupled to a second supply line and a second return line for supplying the reaction fluid from the distribution device to the monitoring cell and for returning the reaction fluid from the monitoring cell to the distribution device, and
a control and regulating device,
wherein:
the distribution apparatus comprises a distribution vessel which houses the distribution device and an electrically controlled pump device configured to pump the reaction fluid,
the distribution device comprises an electrically controlled valve device configured to distribute the reaction fluid to the first and the second supply lines and to the first and the second return lines,
each of the supply lines and the return lines open into the distribution vessel, and
the control and regulating device is configured to electrically control the pump device and the valve device.

2. The monitoring device as claimed in claim 1 , wherein the electrically controlled valve device configured to distribute the reaction fluid comprises a switchable four-way valve, which in a first operating position (“on flow”), connects the first supply line from the reaction vessel to the distribution vessel, directly or indirectly, with the second supply line from the distribution vessel to the monitoring cell and the second return line from the monitoring cell to the distribution vessel, directly or indirectly, with the first return line from the distribution vessel to the reaction vessel,
and which, in a second operating position (“stopped flow”), connects the first supply line from the reaction vessel to the distribution vessel, directly or indirectly, with the first return line from the distribution vessel to the reaction vessel and the second supply line from the distribution vessel to the monitoring cell, directly or indirectly, with the second return line from the monitoring cell to the distribution vessel.

3. The monitoring device as claimed in claim 1 , wherein the electrically controlled pump device configured to pump the reaction fluid comprises a single pump.

4. The monitoring device as claimed in claim 1 , wherein the electrically controlled pump device configured to pump the reaction fluid comprises a transportation path pump, which is fluidly connected to the first supply line from the reaction vessel and pumps reaction fluid through the distribution vessel to the first return line from the distribution vessel to the reaction vessel, and wherein the electrically controlled pump device additionally comprises a measurement path pump, which is fluidly connected to the transportation pump and pumps at least one partial stream of the reaction fluid conveyed by the transportation path pump into the valve device for distributing the reaction fluid to the monitoring cell and to the reaction vessel.

5. The monitoring device as claimed in claim 4 , wherein, in a flow path of the conveyed reaction fluid downstream of the transportation path pump, a first distribution piece is provided, which diverts a partial stream of the conveyed reaction fluid to the measurement path pump and another partial stream of the conveyed reaction fluid to the first return line from the distribution vessel to the reaction vessel, and wherein, in the flow path of the conveyed reaction fluid, a second distribution piece is positioned upstream of the first return line from the distribution device to the reaction vessel, which combines the partial stream of the conveyed reaction fluid to the first return line with another partial stream of the reaction fluid from the monitoring cell exiting the valve device, and provides said combined stream to the first return line from the distribution vessel to the reaction vessel.

6. The monitoring device as claimed in claim 1 , wherein parts of the pump device and of the valve device moistened with the reaction fluid and an entire fluid path of the reaction fluid are composed of chemically inert materials.

7. The monitoring device as claimed in claim 1 , wherein the pump device, the valve device, and an entire fluid path of the reaction fluid are composed of materials that are usable in an operating temperature range of −50° C. to +150° C. or −20° C. to +100° C.

8. The monitoring device as claimed in claim 4 , wherein at least one pump of the electrically controlled pump device configured to pump the reaction fluid is configured to operate at a flow rate of between 10 ml/min and 1,000 ml/min.

9. The monitoring device as claimed in claim 4 , wherein at least one pump of the electrically controlled pump device configured to pump the reaction fluid is configured to operate at a flow rate of between 0.1 ml/min and 10 ml/min.

10. The monitoring device as claimed in claim 1 , wherein the control and regulating device for the electrical control of the pump device and for the electrical control of the valve device is configured to allow volume flow and independent control of the transportation path pump and the measurement path pump, depending on a course of the reaction in the reaction vessel.

11. The monitoring device as claimed in claim 1 , wherein the control and regulating device configured to electrically control the pump device and to electrically control the valve device is configured to allow time-controlled and/or volume-controlled regulation of the valve device and/or the pump device, depending on a course of the reaction in the reaction vessel.

12. The monitoring device as claimed in claim 4 , wherein, in the flow path of the conveyed reaction fluid, sensors are positioned at different, spatially separate sites, and wherein the sensors are configured to detect one or more of: current temperature, current pressure, current pH, or current flow rate of the reaction fluid, wherein the sensors are connected with the control and regulating device configured to electrically control the pump device and to electrically control the valve device, and wherein the control and regulating device is configured to allow one or more of: temperature-controlled, pressure-controlled, pH-controlled, or flow-rate-dependent regulation of the valve device and/or the pump device, depending on a course of the reaction in the reaction vessel.

13. The monitoring device as claimed in claim 1 , wherein the distribution vessel is enclosed in a housing that is constructed in a thermally insulating manner.

14. The monitoring device as claimed in claim 4 , further comprising a thermostat device configured to provide temperature control to an entire flow path of the conveyed reaction fluid from the reaction vessel via the distribution vessel to the monitoring cell and from the monitoring cell via the distribution vessel to the reaction vessel, wherein the control and regulating device configured to electrically control the pump device and to electrically control the valve device is configured to allow temperature control of the thermostat device, dependi

Assignees

• Bruker Biospin Gmbh

Inventors

• Braumann Ernst Ulrich
• Hofmann Martin

Classifications

• G01N24/08

  by using nuclear magnetic resonance (G01N24/12 takes precedence) · CPC title

• G01R33/31

  Temperature control thereof · CPC title

• G01R33/307

  specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer · CPC title

• G01N35/1095

  for supplying the samples to flow-through analysers (for a specific analyser see relevant groups, e.g. under G01N15/00, G01N21/00, G01N27/00, G01N30/00, H01J49/00) · CPC title

• G01N24/085

  Analysis of materials for the purpose of controlling industrial production systems · CPC title