System for automatic sampling, sample digestion, and joining a plurality of sample introduction systems

Patent metadata

Field	Value
Publication number	US-11062893-B2
Application number	US-201916240766-A
Country	US
Kind code	B2
Filing date	Jan 6, 2019
Priority date	Jan 8, 2018
Publication date	Jul 13, 2021
Grant date	Jul 13, 2021

Abstract

Systems and methods for automatic sampling, digestion, and joining a plurality of sample introduction systems of a sample for subsequent analysis by ICP-MS are described. A system embodiment may include: a digestion vessel configured to receive a sample from a pressurized sample source; a shutoff valve configured to control a flow of the sample to the digestion vessel; a first syringe pump configured to introduce a reagent to the sample in the digestion vessel; a thermally-controlled block surrounding the digestion vessel and configured to control the temperature of the digestion vessel, wherein the thermally-controlled block increases the temperature of the digestion vessel to a first set temperature before digestion and wherein the thermally-controlled block decreases the temperature of the digestion vessel to a second set temperature after digestion; a level sensor configured to measure a level of the sample within the digestion vessel; a second syringe pump configured to introduce deionized water to the digestion vessel after digestion, based at least in part on the level measured by the level sensor; and a connector valve configured to receive digested sample from the digestion vessel and transfer the digested sample to an analysis system.

First claim

What is claimed is:

1. A system, comprising:
a digestion vessel configured to receive a sample from a pressurized sample source;
a shutoff valve configured to control a flow of the sample to the digestion vessel;
a first pump configured to introduce a reagent to the sample in the digestion vessel;
a thermally-controlled block surrounding the digestion vessel and configured to control the temperature of the digestion vessel, wherein the thermally-controlled block increases the temperature of the digestion vessel to a first set temperature for a duration of time to permit digestion of at least a portion of the sample within the digestion vessel and wherein the thermally-controlled block decreases the temperature of the digestion vessel to a second set temperature after the duration of time;
a level sensor configured to measure a level of the sample inside the digestion vessel at least after the duration of time;
a second pump configured to introduce deionized water to the digestion vessel, based at least in part on the level measured by the level sensor; and
a connector valve configured to receive digested sample from the digestion vessel and transfer the digested sample to an analysis system.

2. The system of claim 1 , further comprising:
a filtration system configured to filter the digestion sample prior to transfer to the analysis system.

3. The system of claim 1 , further comprising:
a controller coupled to the digestion vessel, the shutoff valve, the first pump, the thermally-controlled block, the level sensor, the second pump, and the connector valve, the controller configured to control at least one of: sampling of fluids, operation of the digestion vessel, or manipulating samples for analysis by the analysis system.

4. The system of claim 1 , wherein the digestion vessel further comprises:
a secondary overflow outlet comprising a leak sensor to monitor flow of fluid through the secondary overflow outlet.

5. The system of claim 1 , further comprising:
an agitation system for managing agitation of the digestion vessel, comprising:
a magnetic stir bar; and
a magnetic stir plate to control rotation of the magnetic stir bar within the digestion vessel.

6. The system of claim 1 , wherein the thermally-controlled block further comprises: a peltier device.

7. The system of claim 1 , further comprising: a sample loop in fluid communication with the connector valve, the sample loop configured to receive at least one of:
the sample pushed by a first pump or a second sample pulled by a second pump.

8. A method, comprising:
controlling a flow of a sample from a pressurized sample source to a digestion vessel via a shutoff valve;
capturing a specific volume of the sample in the digestion vessel;
adding a reagent to the sample in the digestion vessel via a first pump;
increasing a temperature of the digestion vessel to a first set temperature for a set time using a thermally-controlled block to permit digestion of at least a portion of the sample within the digestion vessel;
measuring a level of the sample inside the digestion vessel via a level sensor;
based at least in part on the measured level of the sample inside the digestion vessel, introducing deionized water, via a second pump, to the digestion vessel to return the sample to the specific volume;
actively decreasing the temperature of the digestion vessel to a second set temperature that is less than the first set temperature using the thermally-controlled block; and
transferring the sample from the digestion vessel to an analysis system.

9. The method of claim 8 , further comprising:
filtering the digested sample from the digestion vessel via a filtration system.

10. The method of claim 8 , further comprising:
monitoring a flow of fluid through a secondary outlet port of the digestion vessel via a leak sensor.

11. The method of claim 8 , wherein digesting the sample in the digestion vessel further comprises:
agitating the sample using an agitation system, the agitation system comprising:
a magnetic stir bar; and
a magnetic stir plate to control rotation of the magnetic stir bar within the digestion vessel.

12. The method of claim 8 , wherein the thermally-controller block further comprises a peltier device.

13. The method of claim 8 , further comprising:
receiving, via a sample loop, at least one of: the sample pushed by a first pump or a second sample pulled by a second pump;
wherein the sample loop is in fluid communication with the connector valve.

14. The method of claim 8 , wherein transferring the sample from the digestion vessel to an analysis system further comprises:
drawing, via a third pump, the sample from the digestion system into a sample loop;
pushing, via the third pump, the sample from the sample loop into the filtration system; and
introducing the sample from the filtration system to the connector valve.

15. A system comprising:
a connector valve coupled between at least two sample introduction systems, the connector valve configured to receive a first sample from a first sample introduction system and a second sample from a second sample introduction system, wherein the first sample introduction system comprises:
a digestion vessel configured to receive the first sample from a pressurized sample source;
a shutoff valve configured to control a flow of the first sample to the digestion vessel;
a first pump configured to introduce a reagent to the first sample in the digestion vessel;
a thermally-controlled block surrounding the digestion vessel and configured to control the temperature of the digestion vessel, wherein the thermally-controlled block increases the temperature of the digestion vessel to a first set temperature for a duration of time to permit digestion of at least a portion of the sample within the digestion vessel and wherein the thermally-controlled block decreases the temperature of the digestion vessel to a second set temperature after the duration of time;
a level sensor configured to measure a level of the first sample inside the digestion vessel at least after the duration of time; and
a second pump configured to introduce deionized water to the digestion vessel, based at least in part on the level of the first sample measured by the level sensor;

a sample loop in fluid communication with the connector valve, the sample loop configured to receive the first sample pushed by the first pump and configured to receive the second sample pulled by the second pump; and
an analysis system configured to analyze at least one of: the first sample or the second sample.

16. The analysis system of claim 15 , further comprising an Inductively Coupled Plasma (ICP) Spectrometer, an Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) or an Inductively Coupled Plasma Mass Spectrometer (ICP-MS).

17. The system of claim 15 , further comprising: an agitation system for managing agitation of the digestion vessel, comprising:
a magnetic stir bar; and
a magnetic stir plate to control rotation of the magnetic stir bar within the digestion vessel.

18. The system of claim 15 , wherein the thermally-controlled block comprises: a peltier device.

19. The system of claim 15 , further comprising: a sample loop in fluid communication with the connector valve, the sample loop configured to receive at least one of:
the sample pushed by the first pump or the second sample pulled by the second pump.

20. The system of claim 15 , further comprising:
a controller coupled to the di

Assignees

• Elemental Scientific Inc

Inventors

• Saetveit Nathan
• Field Michael P
• Wiederin Daniel R
• Yost Tyler

Classifications

• B01F35/831

  using one or more pump or other dispensing mechanisms for feeding the flows in predetermined proportion, e.g. one of the pumps being driven by one of the flows (B01F35/832 takes precedence) · CPC title

• B01F31/40

  with an axially oscillating rotary stirrer · CPC title

• B01F35/2215

  Temperature · CPC title

• B01F35/2112

  Level of material in a container or the position or shape of the upper surface of the material · 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