# US 9,435,746 B2 · Multifunctional sol-gel detector for gaseous compounds and detection and trapping methods therewith > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,435,746 B2 - Document ID: US9435746B2 - Status: Granted - Kind: B2 - Application number: 13/992,154 - Filed: 2011-12-14 - Published: 2013-10-24 - Granted: 2016-09-06 - Earliest claimed: 2010-12-16 - Assignees: Commissariat A L'energie Atomique Et Aux Energies Alternatives; Centre National De La Recherche Scientifique (Crns) - Applicants: Thu-Hoa Tran-Thi; Julien Garcia; Thi Dinh Nguyen; Trung-Hieu Nguyen - Inventors: Thu-Hoa Tran-Thi; Julien Garcia; Thi Dinh Nguyen; Trung-Hieu Nguyen - Web page: https://patentgrep.com/patent/US9435746B2 ## CPC - G01N 21/783: {for analysing gases} - G01N 31/224: {for investigating presence of dangerous gases} - Y10T 436/173845: Amine and quaternary ammonium - Y10T 436/177692: Oxides of nitrogen - Y10T 436/19: Halogen containing - 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) - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract The invention relates to a multifunctional detector for gaseous compounds, or mixtures of gaseous compounds, selected from NH2Cl, NHCl2, NCl3, total chlorine, NOx, where x=1 or 2, O3, and X2, where X=Cl, Br, or I, in a sample, said detector including a first sensor including an iodide and a reactive compound selected from starch, amylose, amylopectin, xyloglucan, xylan, chitosan, glycogen, polyvinyl alcohol, cellulose or a cellulose compound, α-cyclodextrin, theobromine, and polypropylene block polymers and polyethylene oxide block polymers, included in a block of sol-gel material that is absorbent in the UV spectrum but not in the visible spectrum. The invention also relates to the uses of said detector. ## Claims ### Claim 1 A multifunctional detector for gaseous compounds or mixtures of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2, where X=Cl, Br or I in a sample, said detector comprising a first sensor consisting of i) a block of sol-gel material that absorbs in the UV but not in the visible ii) an iodide and iii) a reactive compound selected from starch, amylose, amylopectin, xyloglucan, xylane, chitosan, glycogen, polyvinyl alcohol or a polyvinyl alcohol compound, cellulose or a cellulose compound, α-cyclodextrin, theobromine and block polymers of polypropylene oxides and polyethylene oxides, wherein the iodide and the reactive compound are incorporated into the block of sol-gel material. ### Claim 2 (depends on 1) The multifunctional detector as claimed in claim 1, characterized in that in a block of sol-gel material of the first sensor, the iodide represents from 0.0054% to 0.55% by weight of the block. ### Claim 3 (depends on 1) The multifunctional detector as claimed in claim 1, characterized in that in a block of sol-gel material of the first sensor, the reactive compound represents from 0.05% to 0.25% by weight of the block. ### Claim 4 (depends on 1) The multifunctional detector as claimed in claim 1, suitable for gaseous compounds or mixtures of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn where n=1 or 2; O3; and X2 where X=Cl, Br or I in a gaseous sample, said detector further comprising a first compartment containing the first sensor; and a second compartment comprising a second sensor, wherein the second sensor comprises phenol, sodium hydroxide, and sodium nitroprussiate, incorporated into a sol-gel matrix that absorbs in the UV but not in the visible. ### Claim 5 (depends on 4) The multifunctional detector as claimed in claim 4, wherein the first compartment is sub-compartmentalized in order to contact two portions of the gaseous mixture, wherein the first portion of the gaseous mixture contacts a first sub-compartment containing a first sensor and the second portion of the gaseous mixture contacts a second sub-compartment containing a second first sensor, wherein the first portion of the gaseous mixture passes through a filter comprising a neutral silicate matrix impregnated with sulfamic acid to eliminate all the chlorinated species with the exception of NCl3 before contacting the first sub-compartment of the first sensor, said filter being placed upstream of the first sensor. ### Claim 6 (depends on 5) The multifunctional detector as claimed in claim 5, wherein in the filter comprising a neutral silicate matrix, the sulfamic acid represents from 5% to 15% by weight of the total of the silicate and sulfamic acid constituents of the neutral silicate matrix. ### Claim 7 (depends on 5) The multifunctional detector as claimed in claim 5, wherein in the second sensor, the phenol represents from 10% to 25% by weight of the block of sol-gel material. ### Claim 8 (depends on 5) The multifunctional detector as claimed in claim 5, wherein in the second sensor, sodium nitroprussiate represents from 0.01% to 0.25% by weight of the block of sol-gel material. ### Claim 9 (depends on 5) The multifunctional detector as claimed in claim 5, wherein in the second sensor sodium hydroxide represents from 1% to 17% by weight of the block of sol-gel material. ### Claim 10 (depends on 5) A process for detecting gaseous compounds or a mixture of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I contained in a liquid or gaseous sample, comprising exposing the multifunctional detector of claim 5 to a flow of a gas mixture or to a liquid and observing any color change of the blocks of sol-gel material of the first sensor or of the second sensor, and optionally identifying the presence of the gaseous compounds in the sample when a color change is observed. ### Claim 11 (depends on 5) A method for detecting of gaseous compounds or mixtures of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I contained in a gas mixture sample, comprising contacting the multifunctional detector of claim 5 with said gas mixture sample and detecting said compounds with said detector. ### Claim 12 (depends on 4) The multifunctional detector as claimed in claim 4, wherein in the second sensor, the phenol represents from 10% to 25% by weight of the block of sol-gel material. ### Claim 13 (depends on 4) The multifunctional detector as claimed in claim 4, wherein in the second sensor, sodium nitroprussiate represents from 0.01% to 0.25% by weight of the block of sol-gel material. ### Claim 14 (depends on 4) The multifunctional detector as claimed in claim 4, wherein in the second sensor sodium hydroxide represents from 1% to 17% by weight of the block of sol-gel material. ### Claim 15 (depends on 4) A process for detecting gaseous compounds or a mixture of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I contained in a liquid or gaseous sample, comprising exposing the multifunctional detector of claim 4 to a flow of a gas mixture or to a liquid and observing any color change of the blocks of sol-gel material of the first sensor or of the second sensor, and optionally identifying the presence of the gaseous compounds in the sample when a color change is observed. ### Claim 16 (depends on 4) A method for detecting gaseous compounds or mixtures of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I contained in a gas mixture sample, comprising contacting the multifunctional detector of claim 4 with said gas mixture sample and detecting said compounds with said detector. ### Claim 17 (depends on 1) The multifunctional detector as claimed in claim 1, wherein the multifunctional detector further comprises a filter comprising a neutral silicate matrix impregnated with sulfamic acid in order to eliminate all the chlorinated species with the exception of NCl3 from at least a portion of the gaseous compounds or mixtures of gaseous compounds before bringing into contact with the first sensor. ### Claim 18 (depends on 17) The multifunctional detector as claimed in claim 17, wherein in the filter comprising a neutral silicate matrix, the sulfamic acid represents from 5% to 15% by weight of the total of the silicate and sulfamic acid constituents of the neutral silicate matrix. ### Claim 19 (depends on 1) The multifunctional detector as claimed in claim 1, said detector further comprising two first sensors, a first compartment containing one of the two first sensors; and a second compartment containing the other of the two first sensors, wherein the first and second compartments contact two portions of the gaseous mixture, wherein the first portion of the gaseous mixture contacts the first sensor located in the first compartment and the second portion of the gaseous mixture contacts the other first sensor located in the second compartment, wherein the first portion of the gaseous mixture passes through a filter comprising a neutral silicate matrix impregnated with sulfamic acid to eliminate all the chlorinated species with the exception of NCl3 before contacting the first sensor located in the first compartment, said filter being placed upstream of the first sensor. ### Claim 20 (depends on 1) A method for detecting gaseous compounds or mixtures of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I contained in a gas mixture sample, comprising contacting the multifunctional detector of claim 1 with said gas mixture sample and detecting said compounds with said detector. ### Claim 21 (depends on 1) A process for trapping gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I contained in a gas mixture or in a liquid sample, using either the first sensor of claim 1, or a second sensor comprising phenol, sodium hydroxide, and sodium nitroprussiate, incorporated into a sol-gel matrix that absorbs in the UV but not in the visible, wherein said process is conducted when said gas mixture or liquid sample is brought into contact with the first or second sensor, or such a flow is made to circulate over first or second sensor. ### Claim 22 (depends on 1) A system for trapping or detecting gaseous compounds contained in a gas mixture or in a liquid sample, comprising, as a sensor, the multifunctional detector of claim 1, wherein in said detector is further characterized by one or more of the features: (a) in a block of sol-gel material of the first sensor, the iodide represents from 0.0054% to 0.55% by weight of the block; (b) the reactive compound represents from 0.05% to 0.25% by weight of the block, or (c) the multifunctional detector further comprises a filter comprising a neutral silicate matrix impregnated with sulfamic acid in order to eliminate all the chlorinated species with the exception of NCl3 from at least a portion of the gaseous compounds or mixtures of gaseous compounds before bringing into contact with the first sensor. ### Claim 23 (depends on 22) The system of claim 22, wherein said detector further comprises a second type of sensor comprising phenol incorporated in a sol-gel matrix that absorbs in the UV but not in the visible. ### Claim 24 (depends on 23) The system of claim 23, wherein in the block of sol-gel material of the second sensor, the phenol represents from 10% to 25% by weight of the block. ### Claim 25 (depends on 23) The system of claim 23, wherein in the block of sol-gel material of the second sensor, sodium nitroprussiate represents from 0.01% to 0.25% by weight of the block. ### Claim 26 (depends on 23) The system of claim 23, wherein the block of sol-gel material of the second sensor comprises sodium hydroxide which represents from 1% to 17% by weight of the block. ### Claim 27 (depends on 23) The system of claim 23, wherein in the filter comprising a neutral silicate matrix, the sulfamic acid represents from 5% to 15% by weight of the total of the silicate and sulfamic acid constituents of the neutral silicate matrix. ### Claim 28 A process for detecting gaseous compounds or a mixture of gaseous compounds contained in a liquid or gaseous sample comprising: exposing a sample comprising gaseous compounds or mixtures of gaseous compounds selected from NH2Cl; NHCl2; NCl3; total chlorine; NOn, where n=1 or 2; O3; and X2 where X=Cl, Br or I to a multifunctional detector said detector comprising a first sensor consisting of i) a block of sol-gel material that absorbs in the UV but not in the visible ii) an iodide and iii) a reactive compound selected from starch, amylose, amylopectin, xyloglucan, xylane, chitosan, glycogen, polyvinyl alcohol or a polyvinyl alcohol compound, cellulose or a cellulose compound, α-cyclodextrin, theobromine and block polymers of polypropylene oxides and polyethylene oxides, wherein the iodide and the reactive compound are incorporated into the block of sol-gel material, and observing any color change of the block of sol-gel material constituting the first sensor. ### Claim 29 A sol-gel sensor that absorbs in the UV but not in the visible produced by a process consisting of: (a) dissolving in an aqueous solution a reactive compound selected from starch, amylose, amylopectin, xyloglucan, xylane, chitosan, glycogen, polyvinyl alcohol or a polyvinyl alcohol compound, cellulose or a cellulose compound, α-cyclodextrin, theobromine and block polymers of polypropylene oxides and polyethylene oxides; (b) homogenizing the aqueous solution and reactive compound solution of (a); (C) boiling the homogenized solution of (b), and then cooling the boiled solution to ambient temperature (d) adding an alkoxide of formula M(OR)n where M is a metal and R is an alkyl group; (e) adding sodium iodide in solid form; (f) stirring the sol material from (e) in the dark and at ambient temperature; and (g) optionally shaping the sol material from (f) in a desired form. ### Claim 30 A sol-gel sensor that absorbs in the UV but not in the visible produced by a process consisting of: (a) dissolving phenol, sodium nitroprussiate, and sodium hydroxide in an aqueous solution comprising water and methanol; (b) stirring the solution from (a); (c) cooling the solution and adding an alkoxide of formula M(OR), where M is a e and R is an alkyl group to form a sol material; and (d) optionally shaping the sol material from (c) in a desired form.