IP Library Granted Patent US 10,845,313
Granted Patent B2
US 10,845,313 · App. 16/004,189 · Granted Nov 24, 2020

Methods and apparatus for determination of halohydrocarbons

Inventors: Harmesh K. Saini (Santa Clara, CA); Michael J. West (San Jose, CA); Qin Wang (San Jose, CA); James Garvey (San Jose, CA); Paul Rand (San Jose, CA); Mark Angelo (San Jose, CA); David Johnston (San Jose, CA); Robert Ormond (San Jose, CA); Ye Han (San Jose, CA)
Assignee: AMS Trace Metals, Inc.
G01N21/78G01N33/1826G01N21/75G01N33/18Y10T436/19Y10T436/193333
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Quick Facts
Patent No.
US 10,845,313
App. No.
16/004,189
Granted
Nov 24, 2020
Kind
B2
Abstract

A real-time, on-line method and analytical system for determining halohydrocarbons in water which operate by (1) extracting on-line samples; (2) purging volatile halohydrocarbons from the water (e.g., with air or nitrogen); (3) carrying the purge gas containing the analytes of interest over a porous surface where the analytes are adsorbed; (4) recovering the analytes from the porous surface with heat (thermal desorption) or solvent (solvent elution) to drive the analytes into an organic chemical mixture; (5) generating an optical change (e.g., color change) in dependence upon a reaction involving the analytes and a pyridine derivative; and (6) measuring optical characteristics associated with the reaction to quantify the volatile halogenated hydrocarbon concentration.

Claims (47)

1. An apparatus comprising:

a sampling mechanism to draw water samples from a water supply;

a measurement device to measure halohydrocarbons present in respective ones of the water samples; and

at least one processor to intermittently control the sampling mechanism and the measurement device, so as to automate the drawing of the water samples from the water supply and the measurements of the halohydrocarbons present in the respective ones of the water samples;

wherein the at least one processor is also to intermittently control the measurement device, so as to perform respective, calibration measurements of halohydrocarbons present in samples drawn from the water supply to which a standard, comprising a known quantity of halohydrocarbons, has been added; and

wherein the at least one processor is to calculate halohydrocarbon concentration for each respective one of the water samples, dependent on at least one of the calibration measurements.

2. The apparatus of claim 1 , wherein the at least one processor is to communicate with the sampling mechanism and the measurement device via a wide area network (WAN).

3. The apparatus of claim 1 , wherein the at least one processor is to control the sampling mechanism and the measurement device to obtain the calibration measurement on a periodic basis, wherein the periodic basis is no less frequent than once per month.

4. The apparatus of claim 1 , wherein:

the apparatus further comprises

a medium to receive the water samples and extract halohydrocarbons from the water samples, and

a reaction vessel to receive extracted halohydrocarbons from the medium;

the at least one processor is to cause a reagent to be added to the reaction vessel;

the measurement device is to measure an optical property of a reaction initiated by the addition of the reagent, to measure halohydrocarbons present in respective ones of the water samples.

5. The apparatus of claim 4 , wherein the reagent is a pyridine derivative characterized by a pyridine structure with one or more substitutions of hydrogen at the carbon atoms of the pyridine.

6. The apparatus of claim 1 , wherein the measurement device is to measure a time-based optical property of a reaction involving halohydrocarbons from the respective ones of the water samples.

7. The apparatus of claim 6 , wherein the measurement device is to obtain at least two time-differentiated measurements of the optical property, and wherein the at least one processor is to calculate concentration of a specific, predetermined specie of halohydrocarbons present in respective ones of the water samples, dependent on the at least two time-differentiated measurements of the optical property for the respective one of the water samples.

8. The apparatus of claim 6 , wherein the apparatus comprises a network interface to exchange with a remote destination measurement data representing the concentration of the specific, predetermined specie of halohydrocarbons.

9. The apparatus of claim 1 , wherein the standard comprises at least one of CHCl 3 , CHBrCl 2 , CHBr 2 Cl and CHBr 3 .

10. The apparatus of claim 1 , wherein the apparatus comprises a heating device to heat water samples drawn from the water supply, a source of a gas to be passed through the samples to purge out the halohydrocarbons, a trap having an adsorbent medium to isolate purged halohydrocarbons from the water samples, and fluidic transfer means to fluidically transfer extracted halohydrocarbons from the adsorbent medium to a reaction vessel.

11. The apparatus of claim 10 , further comprising a mechanism to regenerate the trap, wherein the at least one processor is also to intermittently control the mechanism to regenerate the trap in between of measurement of halohydrocarbons present in respective ones of the water samples.

12. A method comprising:

causing a sampling mechanism to draw water samples from a water supply;

causing a measurement device to measure halohydrocarbons present in respective ones of the water samples; and

causing at least one processor to intermittently control the sampling mechanism and the measurement device, so as to automate the drawing of the water samples from the water supply and the measurements of the halohydrocarbons present in the respective ones of the water samples;

wherein the method further comprises causing the at least one processor to also intermittently control the measurement device so as to perform respective, calibration measurements of halohydrocarbons present in samples drawn from the water supply to which a standard, comprising a known quantity of halohydrocarbons, has been added; and

wherein the method further comprises causing the at least one processor to calculate halohydrocarbon concentration for each respective one of the water samples, dependent on at least one of the calibration measurements.

13. The method of claim 12 , wherein the method further comprises causing the at least one processor to communicate with the sampling mechanism and the measurement device via a wide area network (WAN).

14. The method of claim 12 , wherein the method further comprises causing the at least one processor to control the sampling mechanism and the measurement device to obtain the calibration measurement on a periodic basis, wherein the periodic basis is no less frequent than once per month.

15. The method of claim 12 , wherein the method further comprises:

receiving the water samples with a medium and extracting halohydrocarbons from the water samples, and

receiving extracted halohydrocarbons from the medium into a reaction vessel;

causing a reagent to be added to the reaction vessel; and

causing the measurement device to measure an optical property of a reaction initiated by the addition of the reagent, to measure halohydrocarbons present in respective ones of the water samples.

16. The method of claim 15 , wherein the reagent is a pyridine derivative characterized by a pyridine structure with one or more substitutions of hydrogen at the carbon atoms of the pyridine.

17. The method of claim 12 , wherein the method further comprises causing the measurement device to measure a time-based optical property of a reaction involving halohydrocarbons from the respective ones of the water samples.

18. The method of claim 17 , wherein the method further comprises causing the measurement device to obtain at least two time-differentiated measurements of the optical property, and causing the at least one processor to calculate concentration of a specific, predetermined specie of halohydrocarbons present in the respective ones of the water samples, dependent on the at least two time-differentiated measurements of the optical property for the respective one of the water samples.

19. The method of claim 12 , wherein the method further comprise exchanging with a remote destination via a network measurement data representing concentration of a specific, predetermined specie of halohydrocarbons, the measurement data derive from one or more of the measurements.

20. The method of claim 12 , wherein the standard comprises at least one of CHCl 3 , CHBrCl 2 , CHBr 2 Cl and CHBr 3 .

21. The method of claim 12 , wherein the method further comprises causing the at least one processor to initiate a regeneration cycle following measurement of each of the water samples, so as to prepare a measurement apparatus to measure halohydrocarbons present in an ensuing one of the water samples.

22. A method comprising:

causing a sampling mechanism to draw water samples from a water supply;

causing a measurement device to measure amount of a predetermined specie of halohydrocarbons present in respective ones of the water samples, wherein the measurement device is to obtain at least two time-differentiated measurements of an optical property; and

causing at least one processor to intermittently control the sampling mechanism and the measurement device, so as to automate the drawing of the water samples from the water supply and the measurements of the halohydrocarbons present in the respective ones of the water samples;

wherein the method further comprises causing the at least one processor to also intermittently control the measurement device so as to perform respective, calibration measurements of halohydrocarbons present in samples drawn from the water supply to which a standard, comprising a known quantity of halohydrocarbons, has been added;

wherein the standard comprises at least one of CHCl 3 , CHBrCl 2 , CHBr 2 Cl and CHBr 3 ; and

wherein the method further comprises causing the at least one processor to calculate concentration of the predetermined specie of halohydrocarbons for each respective one of the water samples, dependent on at least one of the calibration measurements, and dependent on the at least two time-differentiated measurements of the optical property for the respective one of the water samples.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 8, 2018
From: SAINI, HARMESH K.; WEST, MICHAEL J.; WANG, QIN; GARVEY, JAMES; RAND, PAUL; ANGELO, MARK; JOHNSTON, DAVID; ORMOND, ROBERT
To: BOLT, N.V.
Reel/Frame 046033/0117 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 8, 2018
From: HAN, YE
To: BOLT, N.V.
Reel/Frame 046033/0132 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 8, 2018
From: BOLT N.V.
To: AMS TRACE METALS, INC.
Reel/Frame 046033/0146 →
Continuity (4)
Continuation 14819454 · Aug 6, 2015
Continuation 13640312
Provisional Application 61326717 · Apr 22, 2010
Related Publication 20190079020A1 · Mar 14, 2019