# US 11,029,246 B1 · Colorimetric detection of shale inhibitors and/or salts

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- Number: US 11,029,246 B1
- Document ID: US11029246B1
- Status: Granted
- Kind: B1
- Application number: 17/110,717
- Filed: 2020-12-03
- Granted: 2021-06-08
- Earliest claimed: 2020-03-20
- Assignees: Halliburton Energy Services, Inc.
- Applicants: Halliburton Energy Services, Inc.
- Inventors: Dale E. Jamison; Xiangnan Ye
- Web page: https://patentgrep.com/patent/US11029246B1

## CPC

- G01N 21/25: Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N 1/38: Diluting, dispersing or mixing samples
- G01N 21/78: producing a change of colour
- G01N 31/22: using chemical indicators (G01N31/02 takes precedence)
- G01N 33/2823: {Raw oil, drilling fluid or polyphasic mixtures}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

A method of detecting a shale inhibitor and/or a salt content in a wellbore servicing fluid (WSF), the method comprising determining a water salinity of a wellbore servicing fluid; dosing a known volume of the wellbore servicing fluid into a container; optionally adding a known volume of diluent (e.g., water) and mixing to provide a test sample; combining the test sample with a chromophore specific to the shale inhibitor and/or the salt, respectively, and optionally mixing; measuring the shale inhibitor content and/or the salt content, respectively, of the test sample using colorimetry; reporting the data from the measuring to a computer control system; determining a wellbore servicing fluid treatment based on the measured shale inhibitor content and/or salt content; subjecting the wellbore servicing fluid system to the treatment; and optionally waiting for a waiting time to retest the wellbore servicing fluid system and repeating.

## Claims

### Claim 1

A method of detecting a salt content of a wellbore servicing fluid (WSF) of a wellbore servicing fluid system as described herein, the method comprising:
(a) determining a water salinity of a wellbore servicing fluid;
(b) dosing an aliquot of the wellbore servicing fluid into a container;
(c) combining the aliquot of the wellbore servicing fluid with a detector compound specific to the salt and mixing to provide a detection solution in the container, wherein the detection solution is characterized by at least one absorption peak wavelength in the range of from about 380 nanometers (nm) to about 760 nm;
(d) measuring the salt content of the detection solution using colorimetry by detecting an absorption intensity for the detection solution at a wavelength within about ±20% of the at least one absorption peak wavelength, comparing the absorption intensity of the detection solution at the wavelength within about ±20% of the at least one absorption peak wavelength with a target absorption intensity to determine the amount of salt in the WSF, and comparing the amount of salt in the WSF with a target amount of the salt;
(e) reporting the data from the measuring at (d) to a computer control system;
(f) determining a wellbore servicing fluid treatment based on the salt content and/or a content of shale inhibitors; and
(g) subjecting the wellbore servicing fluid of the wellbore servicing fluid system to the treatment.

### Claim 2 (depends on 1)

The method of claim 1 further comprising:
adding a known volume of diluent and mixing prior to (c); and/or
(h) waiting for a waiting time to retest the wellbore servicing fluid system; and (i) repeating steps (a) through (g) after the waiting time.

### Claim 3 (depends on 1)

The method of claim 1, wherein the wellbore servicing fluid comprises a drilling fluid.

### Claim 4 (depends on 3)

The method of claim 3, wherein the drilling fluid has been recovered from circulation downhole.

### Claim 5 (depends on 3)

The method of claim 3, wherein the wellbore servicing fluid comprises a water based mud (WBM).

### Claim 6 (depends on 3)

The method of claim 3, wherein the wellbore servicing fluid comprises an oil based mud (OBM), and wherein dosing at (b) further comprises separating an aqueous phase from an oil phase, and wherein the aliquot comprises at least a portion of the separated aqueous phase.

### Claim 7 (depends on 1)

The method of claim 1, wherein (d) measuring the salt content using colorimetry at (e) comprises utilizing an analyzer comprising photosensitive dye(s) comprising the chromophore specific to the salt.

### Claim 8 (depends on 1)

The method of claim 1, wherein the salt comprises NaCl, KCl, NaBr, CaCl2, CaBr2, MgCl2, MgBr2, ZnBr2, an acetate salt, sodium acetate, potassium acetate, ammonium chloride (NH4Cl), potassium phosphate, sodium formate, potassium formate, cesium formate, or a combination thereof.

### Claim 9 (depends on 8)

The method of claim 8, wherein the wellbore servicing fluid comprises a brine.

### Claim 10 (depends on 1)

The method of claim 1, wherein the aliquot of the wellbore servicing fluid comprises a solids reduced and/or diluted volume of the wellbore servicing fluid.

### Claim 11

A method of detecting a shale inhibitor content of a wellbore servicing fluid (WSF) of a wellbore servicing fluid system as described herein, the method comprising:
(a) determining a water phase salinity (WPS) of a wellbore servicing fluid;
(b) dosing an aliquot of the wellbore servicing fluid into a container;
(c) combining the aliquot of the wellbore servicing fluid with a detector compound specific to the shale inhibitor and mixing to provide a detection solution in the container, wherein the detection solution is characterized by at least one absorption peak wavelength in the range of from about 380 nanometers (nm) to about 760 nm;
(d) measuring the shale inhibitor content of the detection solution using colorimetry by detecting an absorption intensity for the detection solution at a wavelength within about ±20% of the at least one absorption peak wavelength, comparing the absorption intensity of the detection solution at the wavelength within about ±20% of the at least one absorption peak wavelength with a target absorption intensity to determine the amount of shale inhibitor in the WSF, and comparing the amount of shale inhibitor in the WSF with a target amount of the shale inhibitor;
(e) reporting the data from the measuring at (d) to a computer control system;
(f) determining a wellbore servicing fluid treatment based on the water phase salinity (WPS) from (a) and the content of shale inhibitor from (d); and
(g) subjecting the wellbore servicing fluid of the wellbore servicing fluid system to the treatment.

### Claim 12 (depends on 11)

The method of claim 11 further comprising:
adding a known volume of diluent and mixing prior to (c); and/or
(h) waiting for a waiting time to retest the wellbore servicing fluid system; and (i) repeating steps (a) through (g) after the waiting time.

### Claim 13 (depends on 11)

The method of claim 11, wherein the wellbore servicing fluid comprises a drilling fluid.

### Claim 14 (depends on 13)

The method of claim 13, wherein the drilling fluid has been recovered from circulation downhole.

### Claim 15 (depends on 13)

The method of claim 13, wherein the wellbore servicing fluid comprises a water based mud (WBM).

### Claim 16 (depends on 13)

The method of claim 13, wherein the wellbore servicing fluid comprises an oil based mud (OBM), and wherein dosing at (b) further comprises separating an aqueous phase from an oil phase, and wherein the aliquot comprises at least a portion of the separated aqueous phase.

### Claim 17 (depends on 11)

The method of claim 11, wherein (d) measuring the shale inhibitor content of the detection solution using colorimetry at (d) comprises utilizing an analyzer comprising photosensitive dye(s) comprising the chromophore specific to the shale inhibitor.

### Claim 18 (depends on 11)

The method of claim 11, wherein the shale inhibitor comprises a polymer, a charged polymer, a salt, or a combination thereof.

### Claim 19 (depends on 18)

The method of claim 18, wherein the shale inhibitor comprises a high molecular weight polymer, potassium chloride, sodium chloride, or a combination thereof.

### Claim 20 (depends on 11)

The method of claim 11, wherein the aliquot of the wellbore servicing fluid comprises a solids reduced and/or diluted volume of the wellbore servicing fluid.
