# US 2025/0146918 A1 · Monitoring nanoparticle additives in wellbore treatment fluid using x-ray fluorescence

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- Number: US 2025/0146918 A1
- Document ID: US20250146918A1
- Status: Published application
- Kind: A1
- Application number: 18/388,046
- Filed: 2023-11-08
- Published: 2025-05-08
- Earliest claimed: 2023-11-08
- Assignees: Halliburton Energy Services, Inc.
- Applicants: Halliburton Energy Services, Inc.
- Inventors: Preston Andrew May; Jay Deville; Sandeep Kumar Borra
- Web page: https://patentgrep.com/patent/US20250146918A1

## CPC

- G01N 15/06: Investigating concentration of particle suspensions (by weighing G01N5/00; investigating sedimentation of particle suspensions G01N15/04; investigating individual particles G01N15/10)
- E21B 49/0875: {determining specific fluid parameters}
- E21B 49/088: {combined with sampling}
- G01N 23/223: by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
- B82Y 35/00: Methods or apparatus for measurement or analysis of nanostructures
- G01N 2223/076: X-ray fluorescence
- G01N 2223/652: impurities, foreign matter, trace amounts
- 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)
- E21B: EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

A fluid monitoring system for monitoring a concentration of nanoparticle additives in wellbore treatment fluid using X-ray fluorescence (XRF) can include a preparation unit and an analysis unit. The preparation unit can generate a representative sample of the wellbore treatment fluid by performing a separation process with respect to a sample of the treatment fluid. The analysis unit can chemically analyze the subset of the treatment fluid sample using XRF to generate radiation intensity data of the representative sample. Based on the radiation intensity data, the fluid monitoring system can determine that the concentration of the nanoparticle additives is outside of a predefined range. In response to determining that the concentration of the nanoparticle additives in the representative sample is outside of the predefined range, the fluid monitoring system can perform a mitigation operation to modify the concentration of the plurality of nanoparticle additives to be within the predefined range.

## Claims

### Claim 1

A system comprising:
a fluid monitoring system positionable at a wellsite to monitor a concentration of a plurality of nanoparticle additives in a treatment fluid transportable downhole in a wellbore at the wellsite, the fluid monitoring system comprising:
a preparation unit positionable to generate a representative sample of the treatment fluid; and
an analysis unit positionable to chemically analyze the representative sample using X-ray fluorescence (XRF) to generate radiation intensity data associated with the representative sample;
a processor; and
a memory that comprises instructions executable by the processor for causing the processor to:
receive, from the analysis unit, the radiation intensity data of the representative sample;
determine, based on the radiation intensity data, whether the concentration of the plurality of nanoparticle additives in the representative sample is outside of a predefined range; and
in response to determining that the concentration of the plurality of nanoparticle additives in the representative sample is outside of the predefined range, perform a mitigation operation to modify the concentration of the plurality of nanoparticle additives to be within the predefined range.

### Claim 2 (depends on 1)

The system of claim 1, wherein the analysis unit is transportable as a handheld device, and wherein the handheld device comprises:
a handle positionable for use by an operator of the analysis unit to position the analysis unit;
an interactive element positionable on the handle and selectable by the operator to initiate the analysis unit to chemically analyze the representative sample; and
a display device positionable to output the radiation intensity data of the representative sample that is determinable using XRF.

### Claim 3 (depends on 1)

The system of claim 1, wherein the plurality of nanoparticle additives comprises (i) a core compound and (ii) a shell compound positionable to surround the core compound, and wherein the analysis unit is further usable to determine the concentration of the plurality of nanoparticle additives by targeting an element of the core compound or the shell compound to analyze using XRF.

### Claim 4 (depends on 3)

The system of claim 3, wherein the core compound or the shell compound is a copolymer generatable by polymerizing a first monomer and a second monomer, and wherein the second monomer comprises the element targetable by the analysis unit.

### Claim 5 (depends on 1)

The system of claim 1, wherein the preparation unit is positionable to perform a separation process to separate the representative sample from a sample of the treatment fluid by centrifuging the sample of the treatment fluid to form a supernatant including the plurality of nanoparticle additives, and wherein the supernatant is analyzable by the analysis unit to determine the concentration of the plurality of nanoparticle additives.

### Claim 6 (depends on 1)

The system of claim 1, wherein the preparation unit comprises a filtration system positionable to perform a separation process to separate solid particles in a sample of the treatment fluid from the plurality of nanoparticle additives to form a filtrate as the representative sample, and wherein the filtrate containing the plurality of nanoparticle additives is analyzable by the analysis unit to determine the concentration of the plurality of nanoparticle additives.

### Claim 7 (depends on 1)

The system of claim 1, wherein the preparation unit is positionable to perform a separation process to separate the representative sample from a sample of the treatment fluid by adding a solvent to the sample of the treatment fluid to selectively extract the plurality of nanoparticle additives into the solvent, and wherein the solvent containing the plurality of nanoparticle additives is analyzable by the analysis unit to determine the concentration of the plurality of nanoparticle additives.

### Claim 8

A method comprising:
receiving, from an analysis unit of a fluid monitoring system, radiation intensity data of a representative sample generated by the analysis unit using X-ray fluorescence, the representative sample generated by a preparation unit of the fluid monitoring system by performing a separation process with respect to a sample of a treatment fluid transported downhole in a wellbore;
determining, based on the radiation intensity data, whether a concentration of a plurality of nanoparticle additives in the representative sample is outside of a predefined range; and
in response to determining that the concentration of the plurality of nanoparticle additives in the representative sample is outside of the predefined range, performing a mitigation operation to modify the concentration of the plurality of nanoparticle additives to be within the predefined range.

### Claim 9 (depends on 8)

The method of claim 8, wherein the analysis unit is transported as a handheld device, and wherein the handheld device comprises:
a handle positioned for use by an operator of the analysis unit to position the analysis unit;
an interactive element positioned on the handle and selectable by the operator to initiate the analysis unit to chemically analyze the representative sample; and
a display device that outputs the radiation intensity data of the representative sample that is generated using XRF.

### Claim 10 (depends on 8)

The method of claim 8, wherein the plurality of nanoparticle additives comprises (i) a core compound and (ii) a shell compound surrounding the core compound, and wherein the analysis unit further determines the concentration of the plurality of nanoparticle additives by targeting an element of the core compound or the shell compound to analyze using XRF.

### Claim 11 (depends on 10)

The method of claim 10, wherein the core compound or the shell compound is a copolymer generated by polymerizing a first monomer and a second monomer, and wherein the second monomer comprises the element targeted by the analysis unit.

### Claim 12 (depends on 8)

The method of claim 8, wherein the preparation unit separates the representative sample from the sample of the treatment fluid by centrifuging the sample of the treatment fluid to form a supernatant including the plurality of nanoparticle additives, and wherein the supernatant is analyzed by the analysis unit to determine the concentration of the plurality of nanoparticle additives.

### Claim 13 (depends on 8)

The method of claim 8, wherein the preparation unit comprises a filtration system that separates solid particles in the sample of the treatment fluid from the plurality of nanoparticle additives to form a filtrate as the representative sample, and wherein the filtrate is analyzed by the analysis unit to determine the concentration of the plurality of nanoparticle additives.

### Claim 14 (depends on 8)

The method of claim 8, further comprising, subsequent to receiving the radiation intensity data of the representative sample:
determining that the concentration of the plurality of nanoparticle additives in the representative sample is within the predefined range; and
forgoing performing the mitigation operation to modify the concentration of the plurality of nanoparticle additives.

### Claim 15

A non-transitory computer-readable medium comprising program code that is executable by a processing device for causing the processing device to:
receive, from an analysis unit of a fluid monitoring system, radiation intensity data of a representative sample generated by the analysis unit using X-ray fluorescence, the representative sample generated by a preparation unit of the fluid monitoring system by performing a separation process with respect to a sample of a treatment fluid transported downhole in a wellbore;
determine, based on the radiation intensity data, whether a concentration of a plurality of nanoparticle additives in the representative sample is outside of a predefined range; and
in response to determining that the concentration of the plurality of nanoparticle additives in the representative sample is outside of the predefined range, perform a mitigation operation to modify the concentration of the plurality of nanoparticle additives to be within the predefined range.

### Claim 16 (depends on 15)

The non-transitory computer-readable medium of claim 15, wherein the representative sample is dehydrated by the preparation unit to form a solid sample, and wherein the radiation intensity data is generated from the solid sample.

### Claim 17 (depends on 15)

The non-transitory computer-readable medium of claim 15, wherein the plurality of nanoparticle additives comprises (i) a core compound and (ii) a shell compound surrounding the core compound, and wherein the concentration of the plurality of nanoparticle additives is determined through targeting an element of the core compound or the shell compound using X-ray fluorescence.

### Claim 18 (depends on 17)

The non-transitory computer-readable medium of claim 17, wherein the core compound or the shell compound is a copolymer generated by polymerizing a first monomer and a second monomer, and wherein the second monomer comprises the element targeted by the analysis unit.

### Claim 19 (depends on 15)

The non-transitory computer-readable medium of claim 15, wherein the representative sample comprises a supernatant of the sample of the treatment fluid generated by the preparation unit by centrifuging the sample of the treatment fluid, and wherein the supernatant is analyzed by the analysis unit to determine the concentration of the plurality of nanoparticle additives.

### Claim 20 (depends on 15)

The non-transitory computer-readable medium of claim 15, wherein the program code is further executable for causing the processing device to, subsequent to receiving the radiation intensity data of the representative sample:
determine that the concentration of the plurality of nanoparticle additives in the representative sample is within the predefined range; and
forgo performing the mitigation operation to modify the concentration of the plurality of nanoparticle additives.
