Detection of trace amounts of perchlorate using SERS-active capture matrices

Patent metadata

Field	Value
Publication number	US-9470671-B1
Application number	US-201514719114-A
Country	US
Kind code	B1
Filing date	May 21, 2015
Priority date	May 21, 2015
Publication date	Oct 18, 2016
Grant date	Oct 18, 2016

Abstract

A perchlorate detector comprising: surface-enhanced Raman spectroscopy (SERS)-active, magnetic, capture matrices that are selective for perchlorate, wherein the capture matrices are designed to be added to a sample solution; a detection chamber configured to hold the sample solution and the capture matrices; a selectively engageable magnet assembly coupled to the detection chamber such that when the magnet assembly is engaged or disengaged the capture matrices are respectively confined or not confined to a confinement region of the detection chamber; and a Raman spectrometer optically aligned with the confinement region of the detection chamber and configured to interrogate the capture matrices when the magnet assembly is engaged in order to detect and determine a concentration of perchlorate bound to the capture matrices.

First claim

We claim:

1. A perchlorate detector comprising:
surface-enhanced Raman spectroscopy (SERS)-active, magnetic, capture matrices that are selective for perchlorate, wherein the capture matrices are designed to be added to a sample solution;
a detection chamber configured to hold the sample solution and the capture matrices wherein the detection chamber comprises a confinement region having an indentation;
a selectively engageable magnet assembly coupled to the detection chamber such that when the magnet assembly is engaged or disengaged the capture matrices are respectively confined or not confined to the confinement region of the detection chamber;
a Raman spectrometer optically aligned with the confinement region of the detection chamber and configured to interrogate the capture matrices when the magnet assembly is engaged in order to detect and determine a concentration of perchlorate bound to the capture matrices; and
a water reservoir hydraulically coupled to the indentation via a valve such that when the valve is open and the magnetic assembly is disengaged water enters the indentation and flushes the capture matrices out of the indentation.

2. The perchlorate detector of claim 1 , further comprising a mixer operatively coupled to the detection chamber and configured to mix the capture matrices and the sample solution so as to increase interaction between the sample solution and the capture matrices to increase capture efficiency.

3. The perchlorate detector of claim 2 , wherein the mixer is an agitator.

4. The perchlorate detector of claim 2 , wherein the mixer is a vortex mixer.

5. The perchlorate detector of claim 2 , wherein the mixer is a folded flow inline mixer.

6. The perchlorate detector of claim 2 , further comprising a conductivity meter operatively coupled to the detection chamber and configured to measure a conductivity of the sample solution.

7. The perchlorate detector of claim 1 , wherein the capture matrices are Ag/2-dimethylaminoethanethiol hydrochloride (DMA) nanoparticles immobilized on amine- or thiol-derivatized magnetic microparticles.

8. The perchlorate detector of claim 1 , wherein the indentation has a shape that is selected from the group consisting of conical, ovoid, and spherical.

9. The perchlorate detector of claim 1 , wherein the detection chamber is a v-shaped channel.

10. The perchlorate detector of claim 1 , wherein the detection chamber is a tube having a round cross-section.

11. A perchlorate detection method comprising the following steps:
mixing a sample solution with surface-enhanced Raman spectroscopy (SERS)-active, magnetic, capture matrices that are selective for perchlorate to create a mixed suspension;
containing the mixed suspension in a detection chamber;
engaging a magnet assembly to confine the capture matrices to a confinement region of the detection chamber;
interrogating the capture matrices confined to the confinement region with a Raman spectrometer that is optically aligned with the confinement region in order to detect and determine a concentration of perchlorate bound to the capture matrices; and
disengaging the magnet assembly and opening a valve to allow water from a water reservoir that is hydraulically coupled to the confinement region to flush the capture matrices out of the confinement region.

12. The method of claim 11 , further comprising the step of testing the mixed suspension for chloride ions.

13. The method of claim 12 , wherein the step of testing the mixed suspension for chloride ions comprises measuring a conductivity of the mixed suspension and estimating a concentration of chloride ions in the mixed suspension based on the measured conductivity.

14. The method of claim 13 , further comprising the step of correcting a perchlorate peak area in light of the estimated concentration of chloride ions in the mixed suspension.

15. The method of claim 14 , wherein the step of correcting the perchlorate peak area is performed according to the following equation: A=A 0 −((VC)/(K+C)), where A and A 0 are respectively the perchlorate peak area in the presence and absence of background ions, C is the concentration of background chloride ions in ppm; and V and K are constants obtained through curve fitting.

16. The method of claim 12 , further comprising the steps of:
using solid phase extraction to remove chloride ions from the sample solution before the sample solution is mixed with the capture matrices; and
measuring a remaining concentration of chloride using a chloride ion selective electrode after the sample solution and capture matrices are mixed.

17. The method of claim 11 , further comprising the step of collecting the capture matrices for verification after they have been interrogated.

18. The method of claim 11 , wherein the steps are performed without using reagents.

Assignees

• Us Navy
• Us Navy

Inventors

• Boss Pamela A
• Putnam Michael D

Classifications

• G01N27/333

  Ion-selective electrodes or membranes (glass electrodes G01N27/36) · CPC title

• G01N21/658

  enhancement Raman, e.g. surface plasmons · CPC title

• G01N33/182 Primary

  Specific anions in water · CPC title

• G01N2021/651

  Cuvettes therefore · CPC title