Stop-flow analytical systems and methods

• US 8,748,191 B2
• Filed: 08/02/2010
• Issued: 06/10/2014
• Est. Priority Date: 08/02/2010
• Status: Active Grant

• Current Assignee: Ecolab USA Incorporated (Ecolab, Inc.)
• Original Assignee: Ecolab USA Incorporated (Ecolab, Inc.)
• Inventors: Kraus, Paul R., Christensen, William M.
• Primary Examiner(s): Soderquist, Arlen
• Application Number:
  US12/848,450
• Publication Number:
  US 20120028364A1
• Time in Patent Office: 1,408 Days
• Field of Search: 422 62- 63, 422/67, 422 81- 82, 422/82.05, 422 8208- 8209, 422501-505, 436/129, 436/135, 436/164, 436/166, 436171-172, 436/174, 436179-180
• US Class Current: 436/135
• CPC Class Codes: G01N 2001/386 Other diluting or mixing processes
• CPC Class Codes: G01N 2021/8405 Application to two-phase or mixed materials, e.g. gas dissolved in liquids
• CPC Class Codes: G01N 2035/00465 Separating and mixing arrangements
• CPC Class Codes: G01N 21/31 Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry G01N21/72 takes precedence
• CPC Class Codes: G01N 21/84 Systems specially adapted for particular applications
• CPC Class Codes: G01N 35/1095 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 Class Codes: Y10T 436/20 Oxygen containing
• CPC Class Codes: Y10T 436/201666 Carboxylic acid
• CPC Class Codes: Y10T 436/206664 Ozone or peroxide
• CPC Class Codes: Y10T 436/25 including sample preparation
• CPC Class Codes: Y10T 436/25625 Dilution
• CPC Class Codes: Y10T 436/2575 Volumetric liquid transfer

Abstract

Analytical systems and methods are provided for simultaneously dispensing metered volumes of fluids at different rates and mixing the fluids to generate a mixed sample having the fluids in proportion to the different rates at which they were dispensed. In some cases two or more of the fluids are premixed prior to mixing with other fluids. In some cases a use composition and diluent are simultaneously dispensed at different rates and premixed to form a diluted sample. One or more reagents may be mixed with the diluted sample and the sample mixture can be analyzed to determine characteristics of the use composition.

Claims

1. A stop-flow analytical system, comprising:

a sample pump coupled with a sample input port that allows the sample pump to be coupled to a working source of a use composition having concentrations of one or more substances;

a first reagent pump coupled with a first reagent input port that allows the first reagent pump to be coupled with a source of a first reagent;

a diluent pump coupled with a diluent input port that allows the diluent pump to be coupled with a source of a diluent;

a pre-mixer coupled to the sample pump and the diluent pump, the pre-mixer configured to mix together a finite sample of the use composition delivered by the sample pump and a finite volume of the diluent delivered by the diluent pump, resulting in a diluted sample;

a mixer coupled to the first reagent pump and the pre-mixer, the mixer configured to mix together a finite volume of the first reagent delivered by the first reagent pump and the diluted sample received from the pre-mixer, resulting in a sample mixture;

an optical sensor coupled to the mixer, the optical sensor comprising an optical cell that receives the sample mixture from the mixer, the optical sensor configured to obtain response data from the sample mixture indicative of the concentrations of the one or more substances within the use composition;

a stop-flow mechanism coupled to the optical sensor and configured to stop the flow of the sample mixture while the sample mixture is within the optical cell of the optical sensor; and

a rinse bypass line coupling the diluent input port to the mixer while bypassing the pre-mixer.

2. The analytical system of claim 1, wherein the pre-mixer is a static mixer.

3. The analytical system of claim 2, wherein the static mixer is a piece of tubing with internal baffles, a knotted reactor, a reaction coil, an open tubular reactor, or a serpentine mixing device.

4. The analytical system of claim 1, wherein the pre-mixer is a laminar flow mixer.

5. The analytical system of claim 1, wherein the rinse bypass line couples the diluent pump directly to the mixer.

6. The analytical system of claim 1, further comprising a second reagent pump coupled with a second reagent input port that allows the second reagent pump to be coupled with a source of a second reagent, wherein the mixer is further coupled to the second reagent pump and configured to mix together a finite volume of the second reagent delivered by the second reagent pump with the volumes of the first reagent and the diluted sample.

7. The analytical system of claim 6, wherein the sample pump is coupled to a working source of a use composition having concentrations of one or more substances, and wherein the one or more substances comprise a peracid and a peroxide.

8. The analytical system of claim 7, wherein

the first reagent pump is coupled with a source of a first reagent via the first reagent input port;

the second reagent pump is coupled with a source of a second reagent via the second reagent input port; and

the first reagent comprises an iodide solution with a pH adjusted to an alkaline range and the second reagent comprises an acid or an acidic buffer.

9. The analytical system of claim 8, wherein the first reagent comprises potassium iodide and the second reagent comprises acetic acid.

10. The analytical system of claim 1, wherein the sample pump, the first reagent pump, and the diluent pump each comprise a micropump.

11. The analytical system of claim 1, wherein the sample pump, the first reagent pump, and the diluent pump each comprise a syringe pump having a plunger.

12. The analytical system of claim 11, further comprising a first reagent valve selectively coupling the first reagent pump with the first reagent input port and the mixer, a sample valve selectively coupling the sample pump with the sample input port and the pre-mixer, and a diluent valve selectively coupling the diluent pump with the diluent input port and the pre-mixer.

13. The analytical system of claim 12, wherein the diluent valve also selectively couples the diluent pump with the rinse bypass line coupled to the mixer.

14. The analytical system of claim 11, further comprising an asynchronous actuator mechanically coupled to each of the plungers of the sample pump, the first reagent pump and the diluent pump and configured to simultaneously drive at least two of the plungers of the sample pump, the first reagent pump, and the diluent pump at different rates.

15. The analytical system of claim 14 wherein the asynchronous actuator comprises a driving mechanism, a sample lever, a first reagent lever, and a diluent lever, the levers coupled at a first end to the driving mechanism and at a second end to the plungers of the sample pump, the first reagent pump, and the diluent pump, respectively, wherein actuation of the driving mechanism simultaneously displaces the first end of each of the levers by a respective driving distance and the second end of each of the plurality of levers by a respective plunger distance.

16. The analytical system of claim 15, wherein the driving distance of each of the levers is the same and the plunger distance of at least two of the levers is different.

17. The analytical system of claim 1, further comprising a processor coupled to the optical sensor, the processor programmed with instructions for determining the concentrations of the one or more substances based on the response data and instructing a use composition controller to modify or replace the use composition based on the determined concentrations of the one or more substances.

18. An analytical system, comprising:

sample pumping means coupled with a sample input port that allows the sample pumping means to be coupled to a working source of a use composition having concentrations of one or more substances;

first reagent pumping means coupled with a first reagent input port that allows the first reagent pumping means to be coupled with a source of a first reagent;

second reagent pumping means coupled with a second reagent input port that allows the second reagent pumping means to be coupled with a source of a second reagent;

diluent pumping means coupled with a diluent input port that allows the diluent pumping means to be coupled with a source of a diluent;

pre-mixing means coupled to the sample pumping means and the diluent pumping means, for mixing together a finite sample of the use composition delivered by the sample pumping means and a finite volume of the diluent delivered by the diluent pumping means, resulting in a diluted sample;

mixing means coupled to the first reagent pumping means, the second reagent pumping means, and the pre-mixing means, for mixing together a finite volume of the first reagent delivered by the first reagent pumping means, a finite volume of the second reagent delivered by the second reagent pumping means, and the diluted sample received from the pre-mixing means, resulting in a sample mixture;

optical sensing means coupled to the mixing means for receiving the sample mixture from the mixing means and obtaining response data from the sample mixture indicative of the concentrations of the one or more substances within the use composition; and

stop-flow means coupled to the optical sensing means for stopping the sample mixture while obtaining the response data from the sample mixture.

19. The analytical system of claim 18, further comprising a rinse bypass line coupling the diluent pumping means directly to the mixing means.

20. The analytical system of claim 18, wherein the one or more substances comprise a peracid and a peroxide.

21. The analytical system of claim 20, wherein the first reagent comprises an iodide solution with a pH adjusted to an alkaline range and the second reagent comprises an acid or an acidic buffer.

22. The analytical system of claim 18, further comprising driving means mechanically coupled to each of the sample pumping means, the first reagent pumping means, the second reagent pumping means, and the diluent pumping means for driving at least two of the sample pumping means, the first reagent pumping means, the second reagent pumping means, and the diluent pumping means at different rates.

23. The analytical system of claim 18, further comprising processing means coupled to the optical sensing means for determining the concentrations of the one or more substances based on the response data and instructing a use composition controller to modify or replace the use composition based on the determined concentrations of the one or more substances.

24. A method for determining concentrations of a peracid and/or a peroxide within a use composition, the method comprising:

receiving with a sample pump a use composition having concentrations of a peracid and/or a peroxide from a working source of the use composition;

receiving with a first reagent pump a first reagent;

receiving with a second reagent pump to a second reagent;

receiving with a diluent pump a diluent;

simultaneously actuating the sample pump, the first reagent pump, the second reagent pump, and the diluent pump to dispense a finite sample of the use composition, a finite volume of the first reagent, a finite volume of the second reagent, and a finite volume of the diluent;

pre-mixing the sample of the use composition and the volume of the diluent to form a diluted sample;

mixing the volumes of the first reagent and the second reagent with the diluted sample to form a mixed sample;

stopping the mixed sample within an optical cell of an optical sensor;

obtaining optical response data from the mixed sample while the mixed sample is stopped within the optical cell of the optical sensor, the response data indicative of the concentrations of the peracid and/or the peroxide; and

determining the concentrations of the peracid and/or peroxide based on the optical response data.

25. The method of claim 24, wherein the first reagent comprises an iodide solution with a pH adjusted to an alkaline range and the second reagent comprises an acid or an acidic buffer.

26. The method of claim 24, further comprising simultaneously actuating the sample pump, the first reagent pump, the second reagent pump, and the diluent pump to simultaneously draw the sample of the use composition, the volume of the first reagent, the volume of the second reagent, and the volume of the diluent from their respective sources.

27. The method of claim 26, further comprising selectively coupling the sample pump to a pre-mixer after drawing the sample of the use composition, selectively coupling the diluent pump to the pre-mixer after drawing the volume of the diluent, selectively coupling the first reagent pump to a mixer after drawing the volume of the first reagent, and selectively coupling the second reagent pump to the mixer after drawing the volume of the second reagent.

28. The method of claim 27, further comprising rinsing the mixer with the diluent.

29. The method of claim 26, further comprising flushing a sample line coupled between the source of the use composition and the sample pump before drawing the sample of the use composition.

30. The method of claim 24, further comprising adding a peracid concentrate composition to the use composition when the peracid concentration is determined to be below a minimum peracid threshold concentration.

31. The method of claim 24, further comprising generating a new use composition when the peroxide concentration is determined to be above a maximum peroxide threshold concentration.

32. The method of claim 24, further comprising dispensing at different rates at least two of the volume of the first reagent, the volume of the second reagent, the sample of the use composition, and the volume of the diluent.

33. The method of claim 32, wherein the first reagent pump, the second reagent pump, the sample pump, and the diluent pump each comprise a syringe pump having a plunger, and further comprising actuating the plungers of at least two of the first reagent pump, the second reagent pump, the sample pump, and the diluent pump at different rates with a single driving mechanism.

34. The method of claim 24, further comprising coupling the sample pump to a working source of the use composition and coupling the diluent pump to a source of the diluent.