Detection of organic halide compounds using close loop flow assisted electro-enhanced solid-phase microextraction

Patent metadata

Field	Value
Publication number	US-10429282-B2
Application number	US-201916392369-A
Country	US
Kind code	B2
Filing date	Apr 23, 2019
Priority date	Aug 20, 2015
Publication date	Oct 1, 2019
Grant date	Oct 1, 2019

Abstract

A method for detecting and quantifying haloether contamination in aqueous samples. A flow state is artificially induced upon an aqueous sample and a solid phase microextraction (SPME) fiber, upon which an electric potential is applied, is exposed to the flowing aqueous sample in direct immersion mode. Halide ions liberated from electrophoretically dehalogenated haloether compounds contained in the aqueous sample are absorbed upon the SPME fiber, then later desorbed at a gas chromatograph, separated into individual halide ions and analyzed by mass spectrometry. Effects of various parameters such as absorption time, sample pH, salt content, applied voltage, SPME fiber type, flow rate and background matrix are also described.

First claim

The invention claimed is:

1. A method for detecting and quantifying one or more haloether compounds in an aqueous sample, comprising:
inducing a flow state to the aqueous sample to form a flowing aqueous sample, wherein the aqueous sample is confined to a sample system comprising a sample container, an extraction vial, a pump, and tubing fluidly connecting the sample container, the extraction vial and the pump, and the flow state is a continuous flow of the aqueous sample in the sample system;
immersing a fiber and an electrode into the flowing aqueous sample, wherein the fiber and the electrode are disposed in the extraction vial;
applying a negative voltage to the fiber and a positive voltage to the electrode while the fiber is in contact with the flowing aqueous sample to adsorb the one or more haloether compounds onto the fiber;
removing the fiber from the flowing aqueous sample and thermally desorbing the one or more haloether compounds from the fiber in an injection port of a gas chromatograph-mass spectrometer (GC-MS);
subjecting the one or more haloether compounds to GC-MS analysis to detect and determine a concentration of the one or more haloether compounds,
wherein the aqueous solution has a pH of 2; and
wherein the one or more haloether compounds are selected from the group consisting of chlorophenyl phenyl ether and bromophenyl phenyl ether.

2. The method of claim 1 , wherein the flowing aqueous sample has a flow rate of 10-100 mL min −1 .

3. The method of claim 1 , wherein the fiber is selected from the group consisting of a polydimethylsiloxane (PDMS) fiber, a polyacrylate (PA) fiber, a carbonwax/divinylbenzene (CW/DVB) fiber, a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber, a carboxen/polydimethylsiloxane (CAR/PDMS) fiber, a divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber, a carbowax-polyethylene glycol (CW/PEG) fiber and a carbowax-templated resin (TPR) fiber.

4. The method of claim 1 , wherein the fiber has a thickness of 30-85 μm.

5. The method of claim 1 , wherein the electrode is made of at least one material selected from the group consisting of palladium, platinum, gold, silver, iridium, rhodium, graphite and an intrinsically conducting polymer.

6. The method of claim 1 , wherein the immersing is carried out for 5-15 min at 20-40° C.

7. The method of claim 1 , where the negative voltage applied is −50 V to −10 V and the positive voltage applied is +10 V to +50 V.

8. The method of claim 1 , wherein the aqueous sample has a volume of 25-200 mL.

9. The method of claim 1 , wherein the one or more haloether compounds are present in the aqueous sample at a concentration of 0.05-200 μg L −1 .

10. The method of claim 1 , wherein the thermally desorbing is carried out at 250-300° C. for 2-10 min in the injection port of the GC-MS.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Basheer Chanbasha
• Alsharaa Abdulnaser Khaled

Classifications

• G01N2030/884

  organic compounds · CPC title

• G01N2001/4038

  electric methods, e.g. electromigration, electrophoresis, ionisation · CPC title

• G01N27/447

  using electrophoresis · CPC title

• Y10T436/193333

  In aqueous solution · CPC title

• G01N2030/062

  extracting sample from raw material · CPC title