US 10,379,091 B2Granted

Automatic titrator

AssigneeEcolab USA Inc.

InventorsPaul R. Kraus, Robert Ryther

Life of this patent

Estimating the term…

Abstract

The present invention generally relates to continuous methods quantifying a target analyte concentration in a process solution. These methods are continuous automated titration methods that use titration chemistries to measure the target analyte concentration in the process solution. The method steps provide for efficient and robust automated titration methods for a variety of target analytes.

Claims13

Dependent claims

A method for quantification of a target analyte concentration in a process solution comprising:

(a) inputting a low estimated target analyte concentration, a high estimated target analyte concentration, and a maximum integer value for a data counter,
(b) setting the data counter to 1,
(c) calculating a first target analyte concentration by dividing the sum of the low estimated target analyte concentration and the high estimated target analyte concentration by 2,
(d) calculating a first target analyte flow rate based on the first target analyte concentration and introducing a titrant at the first target analyte flow rate,
(e) measuring a first target analyte signal value that correlates to an actual target analyte concentration,
(f) comparing the first target analyte signal value to a threshold target analyte signal value and a maximum target analyte signal value, and if the first target analyte signal value is between the threshold target analyte signal value and the maximum target analyte signal value, entering the first target analyte concentration and the first target analyte signal value as a first data pair into a data array,
(g) if the first data pair is entered into the data array, then increasing the data counter by 1, or if the first data pair is not entered into the data array, repeating steps (c) to (f) with the data counter at the same value,
(h) calculating a next target analyte concentration using the equation:
C
l
+
1
=
C
l
+
C
max
-
C
min
n
(
1
)
where n is the maximum integer value for the data counter, Cl+1 is the next target analyte concentration, Cl is a previous target analyte concentration, Cmax is the high estimated target analyte concentration or a concentration calculated from equation 3 and Cmin is the low estimated target analyte concentration or a concentration calculated from equation 4, wherein if the next target analyte concentration, Cl+1, is greater than Cmax, then Cl+1 is set to equal Cmin,
(i) calculating a next target analyte flow rate based on the next target analyte concentration and introducing a titrant at the next target analyte flow rate,
(j) measuring a next target analyte signal value that correlates to the actual target analyte concentration,
(k) comparing the next target analyte signal value to a threshold target analyte signal value and a maximum target analyte signal value, and if the next target analyte signal value is between the threshold target analyte signal value and the maximum target analyte signal value, entering the next target analyte concentration and the next target analyte signal value as a next data pair into the data array,
(l) if the next data pair is entered into the data array, then increasing the data counter by 1, or if the next data pair is not entered into the data array, repeating steps (i) to (k) with the data counter set to the same value,
(m) repeating steps (h)-(l) until the number of data pairs entered into the data array equals the maximum value for the data counter,
(n) calculating Σx, Σx2,Σy, Σy2, and Σxy wherein x is the target analyte concentration and y is the signal value for each data pair,
(o) calculating SXX, SYY, and SXY using the following equations:
SXX
=
Σ
⁢
⁢
x
2
-
(
Σ
⁢
⁢
x
)
2
n
,
(
2
⁢
a
)
SYY
=
Σ
⁢
⁢
y
2
-
(
Σ
⁢
⁢
y
)
2
n
,
⁢
and
(
2
⁢
b
)
SXY
=
Σ
⁢
⁢
xy
+
(
Σ
⁢
⁢
x
)
⁢
(
Σ
⁢
⁢
y
)
n
,
(
2
⁢
c
)
(p) calculating an endpoint concentration at (i) a minimum target analyte signal value when the target analyte concentration is inversely proportional to the target analyte signal value or (ii) a maximum target analyte signal value when the target analyte concentration is directly proportional to the target analyte signal value using the following equation:
C
max
=
Σ
⁢
⁢
x
n
-
(
SXX
SXY
)
·
(
Σ
⁢
⁢
y
n
)
(
3
)
(q) calculating a minimum concentration at (i) a maximum target analyte signal value when the target analyte concentration is inversely proportional to the target analyte signal value or (ii) a minimum target analyte signal value when the target analyte concentration is directly proportional to the target analyte signal value using the following equation:
C
min
=
(
SXX
SXY
)
·
(
A
m
-
Σ
⁢
⁢
y
n
+
(
SXY
SXX
)
·
Σ
⁢
⁢
x
n
)
,
(
4
)
wherein Am is the target analyte signal value,
(r) repeating steps (h)-(l) and reassigning data pair designations so the first data pair entered is the first data pair replaced,
(s) repeating steps (n)-(r) until the reaction endpoint is reached or the process is stopped.

165 more elements

Dependencies are inferred from the claim text.

Facts

Application: 15/511,730Filed 17 Sep 2015 · continuation in part
Priority: 17 Sep 2014
Published: US 2019/0033273 A131 Jan 2019
Granted: 13 Aug 2019
Term ends: Not estimatedThe source records don’t support an estimate.

Classification8 codes

G01N 31/166
Using titration: continuous titration of flowing liquids
G01N 35/1002
Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices: reagent dispensers
G06F 17/11
Complex mathematical operations: for solving equations , e.g. nonlinear equations, general mathematical optimization problems
G16C 20/30
Chemoinformatics, i.e. ICT specially adapted for the handling of physicochemical or structural data of chemical particles, elements, compounds…

Family

Application14/489,215Parent of this continuation-in-part · filed 17 Sep 2014
US 2019/0033273 A1Pre-grant publication · published 31 Jan 2019
US 9,766,183 B2Parent of this continuation-in-part
US 2016/0077014 A1Published application
US 10,379,091 B2This patent

From the US filing history. Foreign family members aren’t listed.

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Abstract

A method for quantification of a target analyte concentration in a process solution comprising:

(a) inputting a low estimated target analyte concentration, a high estimated target analyte concentration, and a maximum integer value for a data counter,
(b) setting the data counter to 1,
(c) calculating a first target analyte concentration by dividing the sum of the low estimated target analyte concentration and the high estimated target analyte concentration by 2,
(d) calculating a first target analyte flow rate based on the first target analyte concentration and introducing a titrant at the first target analyte flow rate,
(e) measuring a first target analyte signal value that correlates to an actual target analyte concentration,
(f) comparing the first target analyte signal value to a threshold target analyte signal value and a maximum target analyte signal value, and if the first target analyte signal value is between the threshold target analyte signal value and the maximum target analyte signal value, entering the first target analyte concentration and the first target analyte signal value as a first data pair into a data array,
(g) if the first data pair is entered into the data array, then increasing the data counter by 1, or if the first data pair is not entered into the data array, repeating steps (c) to (f) with the data counter at the same value,
(h) calculating a next target analyte concentration using the equation:
C
l
+
1
=
C
l
+
C
max
-
C
min
n
(
1
)
where n is the maximum integer value for the data counter, Cl+1 is the next target analyte concentration, Cl is a previous target analyte concentration, Cmax is the high estimated target analyte concentration or a concentration calculated from equation 3 and Cmin is the low estimated target analyte concentration or a concentration calculated from equation 4, wherein if the next target analyte concentration, Cl+1, is greater than Cmax, then Cl+1 is set to equal Cmin,
(i) calculating a next target analyte flow rate based on the next target analyte concentration and introducing a titrant at the next target analyte flow rate,
(j) measuring a next target analyte signal value that correlates to the actual target analyte concentration,
(k) comparing the next target analyte signal value to a threshold target analyte signal value and a maximum target analyte signal value, and if the next target analyte signal value is between the threshold target analyte signal value and the maximum target analyte signal value, entering the next target analyte concentration and the next target analyte signal value as a next data pair into the data array,
(l) if the next data pair is entered into the data array, then increasing the data counter by 1, or if the next data pair is not entered into the data array, repeating steps (i) to (k) with the data counter set to the same value,
(m) repeating steps (h)-(l) until the number of data pairs entered into the data array equals the maximum value for the data counter,
(n) calculating Σx, Σx2,Σy, Σy2, and Σxy wherein x is the target analyte concentration and y is the signal value for each data pair,
(o) calculating SXX, SYY, and SXY using the following equations:
SXX
=
Σ
⁢
⁢
x
2
-
(
Σ
⁢
⁢
x
)
2
n
,
(
2
⁢
a
)
SYY
=
Σ
⁢
⁢
y
2
-
(
Σ
⁢
⁢
y
)
2
n
,
⁢
and
(
2
⁢
b
)
SXY
=
Σ
⁢
⁢
xy
+
(
Σ
⁢
⁢
x
)
⁢
(
Σ
⁢
⁢
y
)
n
,
(
2
⁢
c
)
(p) calculating an endpoint concentration at (i) a minimum target analyte signal value when the target analyte concentration is inversely proportional to the target analyte signal value or (ii) a maximum target analyte signal value when the target analyte concentration is directly proportional to the target analyte signal value using the following equation:
C
max
=
Σ
⁢
⁢
x
n
-
(
SXX
SXY
)
·
(
Σ
⁢
⁢
y
n
)
(
3
)
(q) calculating a minimum concentration at (i) a maximum target analyte signal value when the target analyte concentration is inversely proportional to the target analyte signal value or (ii) a minimum target analyte signal value when the target analyte concentration is directly proportional to the target analyte signal value using the following equation:
C
min
=
(
SXX
SXY
)
·
(
A
m
-
Σ
⁢
⁢
y
n
+
(
SXY
SXX
)
·
Σ
⁢
⁢
x
n
)
,
(
4
)
wherein Am is the target analyte signal value,
(r) repeating steps (h)-(l) and reassigning data pair designations so the first data pair entered is the first data pair replaced,
(s) repeating steps (n)-(r) until the reaction endpoint is reached or the process is stopped.

165 more elements

Facts

Application

15/511,730Filed 17 Sep 2015 · continuation in part

Priority

17 Sep 2014

Published

US 2019/0033273 A131 Jan 2019

Granted

13 Aug 2019

Term ends

Not estimatedThe source records don’t support an estimate.

Classification8 codes

G01N 31/166
Using titration: continuous titration of flowing liquids
G01N 35/1002
Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices: reagent dispensers
G06F 17/11
Complex mathematical operations: for solving equations , e.g. nonlinear equations, general mathematical optimization problems
G16C 20/30
Chemoinformatics, i.e. ICT specially adapted for the handling of physicochemical or structural data of chemical particles, elements, compounds…

Family

Application14/489,215Parent of this continuation-in-part · filed 17 Sep 2014

US 2019/0033273 A1Pre-grant publication · published 31 Jan 2019

US 9,766,183 B2Parent of this continuation-in-part

US 2016/0077014 A1Published application

US 10,379,091 B2This patent

From the US filing history. Foreign family members aren’t listed.