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US3966410A Expired / Lapsed US ⏱️ 0.0 years remaining

Group extraction of organic compounds present in liquid samples

Assignee: California Institute of Technology
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Filing: 1974-06-20
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Granted: 1976-06-29
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Expires: 1994-06-20
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Abstract

Abstract An extraction device is disclosed comprising a tube containing a substantially inert, chemically non-reactive packing material with a large surface area to volume ratio. A sample which consists of organic compounds dissolved in a liquid, is introduced into the tube. As the sample passes through the packing material it spreads over the material's large surface area to form a thin liquid film which is held on the packing material in a stationary state. A particular group or family of compounds is extractable from the sample by passing a particular solvent system consisting of a solvent and selected reagents through the packing material. The reagents cause optimum conditions to exist for the compounds of the particular family to pass through the phase boundary between the sample liquid and the solvent of the solvent system. Thus, the compounds of the particular family are separated from the sample liquid and become dissolved in the solvent of the solvent system. The particular family of compounds dissolved in the solvent, representing an extract, exits the tube together with the solvent through the tube's nozzle, while the rest of the sample remains on the packing material in a stationary state. Subsequently, a different solvent system may be passed through the packing material to extract another family of compounds from the remaining sample on the packing material.

Inventors

  • 👤 Vilhelm J. Jahnsen

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-26 12:48
CPC Classifications
G; G01; G01N; G01N1/00; G01N1/28; G01N1/40; G01N1/405; B; B01; B01D; B01D11/00; B01D11/04; B01D15/00; B01D15/08; G01N30/00; G01N2030/009; Y; Y10; Y10S; Y10S436/00; Y10S436/901; Y10T; Y10T436/00; Y10T436/25; Y10T436/25375; Y10T436/255

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 270 words
A method of extracting from a liquid sample, consisting of an aqueous liquid in which chemical compounds are contained, an extract, comprising a selected family of said compounds, the steps comprising providng a substantially hollow tube with inlet and outlet openings and a packing zone therebetween, placing a dry, substantially inert, chemically non-reactive packing material which has a large surface area to volume ratio within said packing zone, directing through said open inlet to said packing material said liquid sample, whereby as it comes in contact with said packing material it spreads out as a thin liquid film over the large surface area of said packing material and is held thereon in a stationary state, and rapidly removing said extract directly from said packing material in bulk out of said outlet opening, without selective fractional migration within the packing zone substantially immediately after the time required for an organic solvent, which is immiscible with the liquid of said sample, to pass through said packing material which is holding said sample as a thin liquid film spread over its large surface area, said step of rapidly removing said extract comprising passing a reagent through said packing material to adjust the pH of said extract in said liquid sample to provide said extract with a partition coefficient value biased very heavily in favor of a solvent, which is immiscible with the liquid of said sample, relative to said sample, passing said solvent, which is immiscible with the liquid of said sample through said packing material, in bulk through said packing material whereby it will exit said outlet opening carrying said extract therewith.
Claim 2
Independent Claim 270 words
A method of extracting from a liquid sample, consisting of an aqueous liquid in which chemical compounds are contained, an extract, comprising a selected family of said compounds, the steps comprising providng a substantially hollow tube with inlet and outlet openings and a packing zone therebetween, placing a dry, substantially inert, chemically non-reactive packing material which has a large surface area to volume ratio within said packing zone, directing through said open inlet to said packing material said liquid sample, whereby as it comes in contact with said packing material it spreads out as a thin liquid film over the large surface area of said packing material and is held thereon in a stationary state, and rapidly removing said extract directly from said packing material in bulk out of said outlet opening, without selective fractional migration within the packing zone substantially immediately after the time required for an organic solvent, which is immiscible with the liquid of said sample, to pass through said packing material which is holding said sample as a thin liquid film spread over its large surface area, said step of rapidly removing said extract comprising passing a reagent through said packing material to adjust the pH of said extract in said liquid sample to provide said extract with a partition coefficient value biased very heavily in favor of a solvent, which is immiscible with the liquid of said sample, relative to said sample, passing said solvent, which is immiscible with the liquid of said sample through said packing material, in bulk through said packing material whereby it will exit said outlet opening carrying said extract therewith.
Claim 3
Dependent Claim 33 words
The method as described in claim 1 wherein said reagent is first passed through to adjust the sample pH to a selected value, and thereafter the solvent is passed through said pH-adjusted sample.
Claim 4
Dependent Claim 19 words
The method as described in claim 1 wherein the reagents and said solvent are simultaneously passed through said sample.
Claim 5
Dependent Claim 166 words
The method as described in claim 1 further including the steps of passing through said packing material after said one family of chemical compounds is extracted, other reagents and at least one solvent which is also immiscible in the liquid of said sample, said subsequently passed through reagents adjusting the pH of the sample remaining on said packing material to a value different from said first value so that the partition coefficient of all the chemical compounds in the remaining sample, belonging to a second family different from the family previously extracted, become heavily in favor of said at least one solvent when compared to the coefficient value in favor of said liquid of said sample and become dissolved in said solvent, said solvent exiting said tube through said outlet and with the extract comprising all the compounds previously present in said sample and belonging to said second family, said sample, except for the removed extracts, remaining as a thin liquid film on said packing material.
Claim 6
Dependent Claim 101 words
The method as described in claim 4 wherein said sample is a biological sample, the liquid thereof is an aqueous liquid, said compounds are organic compounds, said solvent is an organic solvent, and said reagents first adjust the pH to a value in the range between 3 and 5 for extracting the first family of organic compounds comprising the acidic and neutral compounds, and thereafter adjust the pH in the range of 8:5 to extract the second family which includes amphoteric compounds, and thereafter adjust the pH in the range of 12 to extract a third family which includes basic compounds.
Claim 7
Independent Claim 248 words
A method of directly extracting from the liquid sample, consisting of an aqueous liquid in which organic chemical compounds are contained, an extract, comprising a selected family of said compounds, the steps comsisting of providing a substantially hollow tube with inlet and outlet openings and a packing zone therebetween, placing in said packing zone a dry, substantially inert, non-reactive fibrous packing material having a large surface area to volume ratio, applying said liquid sample to said fibrous packing material to spread said liquid sample as a thin liquid film over the large surface area of said fibrous packing material, to be held thereon in a stationary state, and removing an extract from said packing zone directly, in bulk, and without selective fractional migration within said packing zone, substantially immediately after the interval required for a solvent immiscible in the liquid in said sample, to traverse through said packing material over which said thin liquid film is held, comprising passing through said packing material selected reagents and in bulk at least one organic solvent which is immiscible in the aqueous liquid of said sample, said reagent adjusting the pH of said sample to a value at which the part ion coefficients of all of the organic compounds of said sample, belonging to said selected family, become heavily biased in favor of said organic solvent, relative to said aqueous liquid, whereby said selected family of compounds becomes dissolved in said organic solvent and pass out of said packing zone therewith.
Claim 8
Independent Claim 248 words
A method of directly extracting from the liquid sample, consisting of an aqueous liquid in which organic chemical compounds are contained, an extract, comprising a selected family of said compounds, the steps comsisting of providing a substantially hollow tube with inlet and outlet openings and a packing zone therebetween, placing in said packing zone a dry, substantially inert, non-reactive fibrous packing material having a large surface area to volume ratio, applying said liquid sample to said fibrous packing material to spread said liquid sample as a thin liquid film over the large surface area of said fibrous packing material, to be held thereon in a stationary state, and removing an extract from said packing zone directly, in bulk, and without selective fractional migration within said packing zone, substantially immediately after the interval required for a solvent immiscible in the liquid in said sample, to traverse through said packing material over which said thin liquid film is held, comprising passing through said packing material selected reagents and in bulk at least one organic solvent which is immiscible in the aqueous liquid of said sample, said reagent adjusting the pH of said sample to a value at which the part ion coefficients of all of the organic compounds of said sample, belonging to said selected family, become heavily biased in favor of said organic solvent, relative to said aqueous liquid, whereby said selected family of compounds becomes dissolved in said organic solvent and pass out of said packing zone therewith.
Claim 9
Dependent Claim 39 words
The method as described in claim 6 wherein said reagents adjust the pH of said sample to a range of 3:5, whereby said extract definable as a first extract includes the acidic and neutral organic compounds in said sample.
Claim 10
Dependent Claim 155 words
The method as described in claim 7 further including the steps of passing through said packing material after said extract is extracted reagents and at least one solvent which is also immiscible in the liquid of said sample, said subsequently passed through reagents adjusting the pH of the sample remaining on said packing material to a value different from said first value, so that the partition coefficients of all of the components of the compounds in the remaining sample belonging to a second family different from the family previously extracted, become heavily in favor of said solvent relative to the partition coefficient in fabor of said aqueous liquid to become dissolved therein, said solvent exiting said tube through said outlet with the extract comprising all the compounds previously present in said sample and belonging to said second family, said sample, except for the extracted compounds, remaining as a thin liquid film on said packing material.
Claim 11
Independent Claim 295 words
A method of extracting from a liquid sample consisting of an aqueous in which chemical compounds are contained, an extract, comprising a selected family of said compounds, the steps of comprising establishing a packing zone in a substantially hollow tube having an input opening and an output opening on opposite ends thereof, packing said packing zone with a dry, chemically inert, packing material having a large surface area to volume ratio, applying all of said liquid sample to through said input opening to said packing material to physically hold said liquid sample spread as a thin liquid film in a stationary phase over the large surface area of said material, and removing said extract directly from all of said packing material, in bulk, out of said output opening and without selective fractional migration within said packing zone, substantially immediately after the time required for a solvent, which is immiscible with the liquid of said sample, to traverse said packing material over which said liquid film is held, said step of removing said extract from said packing material comprising passing in bulk through said packing material a solvent system including an organic solvent which is immiscible in the liquid of said sample, and a reagent for adjusting the pH of said extract to a value at which the partition coefficient of said extract is so heavily biased in favor of said immiscible solvent that it moves out of solution in said liquid sample and into solution with said solvent, whereby said solvent system passes through and out of said packing zone substantially immediately after traversing the packing material holding said liquid film, removing said extract therewith leaving the remainder of said sample spread as a thin liquid film over the surface area of said packing material.
Claim 12
Independent Claim 295 words
A method of extracting from a liquid sample consisting of an aqueous in which chemical compounds are contained, an extract, comprising a selected family of said compounds, the steps of comprising establishing a packing zone in a substantially hollow tube having an input opening and an output opening on opposite ends thereof, packing said packing zone with a dry, chemically inert, packing material having a large surface area to volume ratio, applying all of said liquid sample to through said input opening to said packing material to physically hold said liquid sample spread as a thin liquid film in a stationary phase over the large surface area of said material, and removing said extract directly from all of said packing material, in bulk, out of said output opening and without selective fractional migration within said packing zone, substantially immediately after the time required for a solvent, which is immiscible with the liquid of said sample, to traverse said packing material over which said liquid film is held, said step of removing said extract from said packing material comprising passing in bulk through said packing material a solvent system including an organic solvent which is immiscible in the liquid of said sample, and a reagent for adjusting the pH of said extract to a value at which the partition coefficient of said extract is so heavily biased in favor of said immiscible solvent that it moves out of solution in said liquid sample and into solution with said solvent, whereby said solvent system passes through and out of said packing zone substantially immediately after traversing the packing material holding said liquid film, removing said extract therewith leaving the remainder of said sample spread as a thin liquid film over the surface area of said packing material.
Claim 13
Independent Claim 305 words
A method of successively extracting from a sample, comprising an aqueous liquid containing different families of chemical compounds, different extracts, each extract including a selected family of said compounds, the steps consisting of providing a substantially hollow tube having an upper inlet end and an opposite outlet end and a packing zone therebetween which is packed with a dry inert chemically non-reactive packing material having a large surface area to volume ratio, pouring said sample into said tube through said inlet and onto said packing material, whereby said sample spreads over the large surface area of said packing material is physically held thereon in a stationary state, successively removing different extracts in bulk, directly from said packing material and out of the outlet end of said tube, without selective fractional migration within the packing zone, substantially immediately after the interval required for a solvent for a particular extract which is immiscible with the liquid of the sample, to travel through the region of said packing material over which said thin liquid film is held, comprising successively passing through said packing material, for each extract to be removed, a selected reagent and in bulk an organic solvent which is immiscible in the aqueous liquid of said sample, said selected reagent adjusting the pH of each extract to a value so that the partition coefficient of all of the compounds within a family which is to be removed, are biased heavily in favor of said immiscible solvent relative to the bias to said aqueous liquid and become dissolved in said organic solvent, whereby each successively added organic solvent, together with the extract dissolved therein passes through said packing zone and out of said inlet end of said tube in bulk, leaving the remainder of said liquid sample dispersed as a thin liquid film on said packing material.
Claim 14
Independent Claim 305 words
A method of successively extracting from a sample, comprising an aqueous liquid containing different families of chemical compounds, different extracts, each extract including a selected family of said compounds, the steps consisting of providing a substantially hollow tube having an upper inlet end and an opposite outlet end and a packing zone therebetween which is packed with a dry inert chemically non-reactive packing material having a large surface area to volume ratio, pouring said sample into said tube through said inlet and onto said packing material, whereby said sample spreads over the large surface area of said packing material is physically held thereon in a stationary state, successively removing different extracts in bulk, directly from said packing material and out of the outlet end of said tube, without selective fractional migration within the packing zone, substantially immediately after the interval required for a solvent for a particular extract which is immiscible with the liquid of the sample, to travel through the region of said packing material over which said thin liquid film is held, comprising successively passing through said packing material, for each extract to be removed, a selected reagent and in bulk an organic solvent which is immiscible in the aqueous liquid of said sample, said selected reagent adjusting the pH of each extract to a value so that the partition coefficient of all of the compounds within a family which is to be removed, are biased heavily in favor of said immiscible solvent relative to the bias to said aqueous liquid and become dissolved in said organic solvent, whereby each successively added organic solvent, together with the extract dissolved therein passes through said packing zone and out of said inlet end of said tube in bulk, leaving the remainder of said liquid sample dispersed as a thin liquid film on said packing material.

References Cited (Backward Citations)

US2733135A Cited
US3625652A Cited
US3776698A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-06-29 1979-12-29 1980-06-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-06-29 1983-12-29 1984-06-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-06-29 1987-12-29 1988-06-29 $7700.00 Window Closed / Lapsed

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