SOLID PHASE SAMPLING DEVICE AND METHODS FOR POINT-SOURCE SAMPLING OF POLAR ORGANIC ANALYTES

• US 20200132653A1
• Filed: 10/25/2018
• Published: 04/30/2020
• Est. Priority Date: 10/25/2018
• Status: Active Grant

• Current Assignee: Battelle Savannah River Alliance LLC
• Original Assignee: Savannah River Nuclear Solutions LLS
• Inventors: BOGGESS, ANDREW J., CRUMP, STEPHEN L., WHITE, THOMAS L.
• Granted Patent: US 11,022,593 B2
• Time in Patent Office: Days
• CPC Class Codes: G01N 1/10 in the liquid or fluent state burettes, pipettes B01L3/02; sampling of ground water E02D1/06; metering by volume of fluids or fluent solid material G01F11/00, G01F13/00
• CPC Class Codes: G01N 1/4044 by chemical techniques; Digestion; Chemical decomposition
• CPC Class Codes: G01N 1/405 by adsorption or absorption
• CPC Class Codes: G01N 2001/1418 Depression, aspiration
• CPC Class Codes: G01N 33/1826 organic contamination in water
• CPC Class Codes: Y02A 20/20 Controlling water pollution; Waste water treatment

Abstract

Sampling devices for sampling an aqueous source (e.g., field testing of ground water) for multiple different analytes are described. Devices include a solid phase extraction component for retention of a wide variety of targeted analytes. Devices include analyte derivatization capability for improved extraction of targeted analytes. Thus, a single device can be utilized to examine a sample source for a wide variety of analytes. Devices also include an isotope dilution capability that can prevent error introduction to the sample analysis and can correct for sample loss and degradation from the point of sampling until analysis as well as correction for incomplete or poor derivatization reactions. The devices can be field-deployable and rechargeable.

Claims

1. A sampling device comprising:

a liquid inlet;

a first layer downstream of the liquid inlet, the first layer comprising a first solid phase extraction medium, the first layer further comprising a first derivatizing agent for a first targeted analyte, reaction between the first derivatizing agent and the first targeted analyte forming a first derivatized analyte;

a second layer downstream of the first layer, the second layer comprising a second solid phase extraction medium, the second layer further comprising an isotopically labeled analogue of the first derivatized analyte; and

a liquid outlet downstream of the second layer.

2. The sampling device of claim 1, wherein the first solid phase extraction medium and/or the second solid phase extraction medium comprises a carbon-based medium, the first solid phase extraction medium and the second solid phase extraction medium being the same or differing from one another.

3. The sampling device of claim 1, wherein the first derivatizing agent comprises a silylation derivatizing agent, an acylation derivatizing agent, or an alkylation derivatizing agent.

4. The sampling device of claim 1, wherein the isotopically labeled analogue of the first derivatized analyte is a carbon-13 labeled analogue.

5. The sampling device of claim 1, wherein the first layer and the second layer are self-supporting removable cartridges.

6. The sampling device of claim 1, further comprising a housing that contains the first layer and the second layer, the housing having a width of from about 1 inch to about 6 inches, a depth of from about 1 inch to about 6 inches, and a height defined between the liquid inlet and the liquid outlet of from about 3 inches to about 10 inches.

7. The sampling device of claim 1, the first layer further comprising a second derivatizing agent for a second targeted analyte, reaction between the second derivatizing agent and the second targeted analyte forming a second derivatized analyte, the second layer further comprising an isotopically labeled analogue for the second derivatized analyte.

8. The sampling device of claim 1, further comprising an isotopically labeled analogue for a third targeted analyte in the second layer.

9. A method for analyzing an aqueous sample comprising:

introducing the aqueous sample into a sampling device, the aqueous sample contacting a first layer in the sampling device, the first layer comprising a first solid phase extraction medium and a first derivatizing agent for a first targeted analyte of the aqueous sample, reaction between the first derivatizing agent and the first targeted analyte forming a first derivatized analyte, the first derivatized analyte being less polar than the first targeted analyte, the aqueous sample subsequently contacting a second layer in the sampling device, the second layer comprising a second solid phase extraction medium and an isotopically labeled analogue of the first derivatized analyte;

allowing a first portion of the aqueous sample to exit the sampling device, a second portion of the aqueous sample being retained on the first and second solid phase extraction media;

following a period of time, eluting the second portion of the aqueous sample from the solid phase extraction media of the device; and

analyzing an eluent thus obtained to determine a concentration of the first targeted analyte in the aqueous sample.

10. The method of claim 9, the first layer further comprising a second derivatizing agent for a second targeted analyte of the aqueous sample, reaction between the second derivatizing agent and the second targeted analyte forming a second derivatized analyte, the second derivatized analyte being less polar than the second targeted analyte, the second layer further comprising an isotopically labeled analogue of the second derivatized analyte, the method further comprising analyzing the eluent to determine a concentration of the second targeted analyte in the aqueous sample.

11. The method of claim 9, the second layer further comprising an isotopically labeled analogue of a third targeted analyte, the method further comprising analyzing the eluent to determine a concentration of the third targeted analyte in the aqueous sample.

12. The method of claim 9, further comprising removing the first and second layers from the sampling device and replacing the first and second layers with a replacement first layer and a replacement second layer.

13. The method of claim 9, further comprising drying the second portion of the aqueous sample.

14. The method of claim 9, wherein the aqueous sample is obtained from a natural source, the method further comprising returning the first portion of the aqueous sample to the natural source.

15. The method of claim 14, wherein the aqueous sample is introduced into the sampling device at the natural source.

16. A method for forming a sampling device comprising:

locating a first layer in a housing downstream of a liquid inlet of the housing, the first layer comprising a first solid phase extraction medium, the first layer further comprising a first derivatizing agent for a first targeted analyte, reaction between the first derivatizing agent and a first targeted analyte forming a first derivatized analyte; and

locating a second layer in the housing downstream of the first layer, the second layer comprising a second solid phase extraction medium, the second layer further comprising an isotopically labeled analogue of the first derivatized analyte.

17. The method of claim 16, wherein the first layer and the second layer are removably held within the housing.

18. The method of claim 16, further comprising loading the first derivatizing agent onto the first layer prior to locating the first layer in the housing.

19. The method of claim 16, further comprising loading the isotopically labeled analogue of the first derivatized analyte onto the second layer prior to locating the second layer in the housing.

20. The method of claim 16, the first layer further comprising a second derivatizing agent, reaction between the second derivatizing agent and a second targeted analyte forming a second derivatized analyte, the second layer further comprising an isotopically labeled analogue of the second derivatized analyte, optionally, the second layer further comprising an isotopically labeled analogue of a third targeted analyte.