# US 8,465,984 B2 · Method of detecting an emulsion in brine > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,465,984 B2 - Document ID: US8465984B2 - Status: Granted - Kind: B2 - Application number: 13/131,979 - Filed: 2010-01-25 - Published: 2011-09-29 - Granted: 2013-06-18 - Earliest claimed: 2009-01-26 - Assignees: M-I L.L.C. - Applicants: Bethicia B. Prasek; Marc A. Churan - Inventors: Bethicia B. Prasek; Marc A. Churan - Web page: https://patentgrep.com/patent/US8465984B2 ## CPC - G01N 33/2823: {Raw oil, drilling fluid or polyphasic mixtures} - G01N 31/22: using chemical indicators (G01N31/02 takes precedence) - 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 The instant disclosure is directed to a method of detecting an emulsion in a turbid brine, the method comprising the steps of disposing an aliquot of the turbid brine into a sample container to produce a test sample; adding one or more drops of a dye solution comprising an oil-soluble dye dissolved in a nonaqueous base fluid to said test sample; and determining the configuration of the dye solution after a period of time on a surface of the test sample, wherein a configuration of the dye solution forming a ring around the perimeter of the sample container at the interface of a wall of the sample container and the turbid brine indicates an emulsion is present in the turbid brine, and wherein a configuration of the dye solution forming a single dot or a plurality of dots on the surface of the turbid brine indicates an emulsion is not present in the turbid brine. ## Claims ### Claim 1 A method of detecting an emulsion in a turbid brine, the method comprising the steps of: disposing an aliquot of the turbid brine into a sample container to produce a test sample; adding one or more drops of a dye solution comprising an oil-soluble dye dissolved in a base oil to said test sample; and determining the configuration of the dye solution after a period of time on a surface of the test sample, wherein a configuration of the dye solution forming a ring around the perimeter of the sample container at the interface of a wall of the sample container and the turbid brine indicates an emulsion is present in the turbid brine, and wherein a configuration of the dye solution forming a single dot or a plurality of dots on the surface of the turbid brine indicates an emulsion is not present in the turbid brine. ### Claim 2 (depends on 1) The method of claim 1, wherein the turbid brine is a completion fluid. ### Claim 3 (depends on 1) The method of claim 1, wherein the turbid brine comprises a halide salt, a formate salt, or a combination thereof. ### Claim 4 (depends on 1) The method of claim 1, wherein the turbid brine comprises sodium chloride, sodium bromide, sodium formate, potassium chloride, potassium bromide, potassium formate, cesium chloride, cesium bromide, cesium formate, calcium chloride, calcium bromide, zinc chloride, zinc bromide, or a combination thereof. ### Claim 5 (depends on 1) The method of claim 1, wherein the base oil comprises mineral oil, diesel fuel, low-aromatic mineral oil, non-aromatic mineral oil, isomerized C16 to C18 alpha-olefins, other nonaqueous fluid, or combinations thereof. ### Claim 6 (depends on 1) The method of claim 1, wherein the test sample comprises a 20 ml scintillation vial filled about halfway with the turbid brine. ### Claim 7 (depends on 1) The method of claim 1, wherein the turbid brine is taken from a well in which a lubricant was used in combination with a completion fluid during drilling of the well. ### Claim 8 (depends on 1) The method of claim 1, wherein the turbid brine has a turbidity of greater then or equal to about 20 NTU. ### Claim 9 (depends on 1) The method of claim 1, wherein the oil-soluble dye comprises a lysochrome, a fat-soluble dye, a solvent dye, or a combination thereof. ### Claim 10 (depends on 1) The method of claim 1, wherein the oil-soluble dye comprises Oil Red O, a Sudan dye, Oil Blue A; Oil Blue N, or a combination thereof. ### Claim 11 A method of detecting an emulsion in a turbid brine, the method comprising the steps of: passing an aliquot of the turbid brine through a 0.1 to 10 micron filter to produce a filtered aliquot; disposing at least a portion of the filtered aliquot into a clean sample container to produce a test sample; adding one or more drops of a dye solution comprising an oil-soluble dye dissolved in a base oil to said test sample; and determining the configuration of the dye solution after a period of time on a surface of the test sample, wherein a configuration of the dye solution forming a ring around the perimeter of the sample container at the interface of a wall of the sample container and the turbid brine indicates an emulsion is present in the turbid brine, and wherein a configuration of the dye solution forming a single dot or a plurality of dots on the surface of the turbid brine indicates an emulsion is not present in the turbid brine. ### Claim 12 (depends on 11) The method of claim 11, wherein the 0.1 to 10 micron filter has a maximum porosity of about 1.6 microns. ### Claim 13 (depends on 11) The method of claim 11, wherein the turbid brine is a completion fluid. ### Claim 14 (depends on 11) The method of claim 11, wherein the turbid brine comprises a halide salt, a formate salt, or a combination thereof. ### Claim 15 (depends on 11) The method of claim 11, wherein the turbid brine comprises sodium chloride, sodium bromide, sodium formate, potassium chloride, potassium bromide, potassium formate, cesium chloride, cesium bromide, cesium formate, calcium chloride, calcium bromide, zinc chloride, zinc bromide, or a combination thereof. ### Claim 16 (depends on 11) The method of claim 11, wherein the base oil comprises mineral oil, diesel fuel, low-aromatic mineral oil, non-aromatic mineral oil, isomerized C16 to C18 alpha-olefins, or combinations thereof. ### Claim 17 (depends on 11) The method of claim 11, wherein the test sample comprises a 20 ml scintillation vial filled about halfway with the turbid brine. ### Claim 18 (depends on 11) The method of claim 11, wherein the turbid brine is taken from a well in which a lubricant was used in combination with a completion fluid during drilling of the well. ### Claim 19 (depends on 11) The method of claim 11, wherein the turbid brine has a turbidity of greater then or equal to about 20 NTU. ### Claim 20 (depends on 11) The method of claim 11, wherein the oil-soluble dye comprises a lysochrome, a fat-soluble dye, a solvent dye, or a combination thereof. ### Claim 21 (depends on 11) The method of claim 11, wherein the oil-soluble dye comprises Oil Red O, a Sudan dye, Oil Blue A; Oil Blue N, or a combination thereof. ### Claim 22 A method of determining the turbidity of a turbid brine, the method comprising the steps of: disposing an aliquot of the turbid brine into a sample container to produce a test sample; adding one or more drops of a dye solution comprising an oil-soluble dye dissolved in a base oil to said test sample; and determining the configuration of the dye solution after a period of time on a surface of the test sample, wherein a configuration of the dye solution forming a ring around the perimeter of the sample container at the interface of a wall of the container and the turbid brine indicates an emulsion is present in the turbid brine, and wherein a configuration of the dye solution forming a single dot or a plurality of dots on the surface of the turbid brine indicates an emulsion is not present in the turbid brine; disposing another aliquot of the turbid brine into a sample container along with an aliquot of an emulsion breaking solvent to produce a centrifuge sample; mixing the centrifuge sample by agitation, shaking, or a combination thereof; centrifuging the centrifuge sample for a period of time sufficient remove solids which may be present in the turbid brine; determining the presence of solids which may have separated from the turbid brine after centrifuging; and removing a portion of the brine from the centrifuge sample and determining the turbidity of the brine. ### Claim 23 (depends on 22) The method of claim 22, wherein the emulsion breaking solvent is ethylene glycol mono-butyl ether. ### Claim 24 (depends on 22) The method of claim 22, wherein an aliquot of the turbid brine is first passed through a 0.1 to 10 micron filter prior to being disposed into the sample container to produce the test sample. ### Claim 25 (depends on 24) The method of claim 24, wherein the 0.1 to 10 micron filter has a maximum porosity of about 1.6 microns. ### Claim 26 (depends on 22) The method of claim 22, wherein the turbid brine is a completion fluid. ### Claim 27 (depends on 22) The method of claim 22, wherein the turbid brine comprises a halide salt, a formate salt, or a combination thereof. ### Claim 28 (depends on 22) The method of claim 22, wherein the turbid brine comprises sodium chloride, sodium bromide, sodium formate, potassium chloride, potassium bromide, potassium formate, cesium chloride, cesium bromide, cesium formate, calcium chloride, calcium bromide, zinc chloride, zinc bromide, or a combination thereof. ### Claim 29 (depends on 22) The method of claim 22, wherein the base oil comprises mineral oil, diesel fuel, low-aromatic mineral oil, non-aromatic mineral oil, isomerized C16 to C18 alpha-olefins, other nonaqueous fluid, or combinations thereof. ### Claim 30 (depends on 22) The method of claim 22, wherein the test sample comprises a 20 ml scintillation vial filled about halfway with the turbid brine. ### Claim 31 (depends on 22) The method of claim 22, wherein the turbid brine is taken from an oil well in which a lubricant was used in combination with a completion fluid during drilling of the oil well. ### Claim 32 (depends on 22) The method of claim 22, wherein the turbid brine has a turbidity of greater then or equal to about 20 NTU. ### Claim 33 (depends on 22) The method of claim 22, wherein the oil-soluble dye comprises a lysochrome, a fat-soluble dye, a solvent dye, or a combination thereof. ### Claim 34 (depends on 22) The method of claim 22, wherein the oil-soluble dye comprises Oil Red O, a Sudan dye, Oil Blue A; Oil Blue N, or a combination thereof.