Patent NL47909C successfully refreshed from Google Patents.
Patent US3607073A successfully refreshed from Google Patents.
US3607073A
Expired / Lapsed
US
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Method and apparatus for analysis of fluid mixtures
Assignee: Texaco Inc
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Filing: 1968-07-22
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Granted: 1971-09-21
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Expires: 1988-07-22
Abstract
Abstract A method and apparatus for continually monitoring a component of a fluid mixture, such as the naphthene content of a hydrocarbon mixture. The apparatus includes a microreactor for subjecting the fluid mixture to a chemical reaction converting, at least in part, a fluid component of the mixture so as to render the fluid component of interest separable from the mixture, and detection means for detecting the fluid component of interest. In a further embodiment a unique computer is provided coupled with the detector for computing the concentration of the fluid component of interest in the fluid mixture. The method of the invention includes reacting the fluid mixture in the aforementioned chemical reaction, and detecting the fluid component of interest. In another version of the method in which the reaction affects more than one component of the mixture converting the affected components to still another component of the mixture, the method includes the further steps of detecting said other component in an unreacted sample of the fluid mixture and generating a signal representative of the concentration in the mixture of the fluid component of interest in accordance with a predetermined relationship between the detected components of the unreacted sample, the reacted sample, and the concentration of the fluid component of interest in the fluid mixture.
Inventors
- 👤 Ralph E Stamm
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 08:38
CPC Classifications
G; G01; G01N; G01N33/00; G01N33/26; G01N33/28; G01N33/2835; G01N30/00; G01N30/02; G01N30/86; G01N30/8603; G01N31/00; G01N30/88; G01N2030/8886; Y; Y10; Y10T; Y10T436/00; Y10T436/21; Y10T436/212
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
21 words
The method of claim 1 wherein said detecting steps (a) and (c) include generating second and third signals representative thereof respectively,
Claim 2
Dependent Claim
191 words
The method of claim 2 wherein said predetermined relationship is determined in accordance with the steps comprising: e. detecting the concentration of said second component in a sample of said reference second fluid mixture and generating a fourth signal representative thereof; f. reacting said sample of said reference second fluid mixture in a chemical reaction converting at least a portion of said first component into said second component, said reaction being performed under substantially the same conditions as said reaction of step (b); g. detecting the concentration of said second component in said sample of said reference second fluid mixture subsequent to said reacting step (f) and generating a fifth signal representative thereof; and h. combining said second, third, fourth and fifth signals in a proportional relationship relatIng the concentration of said second component in said sample of said reference second fluid mixture before and after said reacting step (f) with the concentration of said second component in said sample of said first named fluid mixture before and after said reacting step (b) and with said predetermined concentration of said first component in said sample of said reference second fluid mixture.
Claim 3
Dependent Claim
131 words
The method of claim 3 wherein said second, third, fourth and fifth signals are combined in said step (h) substantially in accordance with the following equation: Y Y1(x2- x1)/(z2- z1) where: Y the concentration of said first component for detection in said first named fluid mixture, Y1 the concentration of said first component in said reference second fluid mixture, z1 the concentration of said second component in said reference second fluid mixture prior to said reaction thereof, z2 the concentration of said second component in said reference second fluid mixture subsequent to said reaction thereof, x1 the concentration of said second component in said first named fluid mixture prior to said reaction thereof, x1 the concentration of said second component in said first named fluid mixture subsequent to said reaction thereof.
Claim 4
Dependent Claim
272 words
The method of claim 4 wherein said first and second fluid mixtures consist essentially of fluid components selected from the group consisting of aromatics, naphthenes, and paraffins, wherein said first fluid component of said fluid mixtures consists essentially of naphthenes, wherein said second component of said fluid mixtures consists essentially of aromatics, wherein said reactions of steps (b) and (f) are performed in the presence of a noble metal catalyst and in the presence of hydrogen for conversion of at least a portion of said naphthenes to aromatics, wherein said method includes the further steps of heating said samples of said first and second fluid mixtures to a temperature in the range of about 200* to 400* C. at least in part during said respective reacting steps (b) and (f), and wherein each of said detecting steps (a), (c) and (g) include the steps of; introducing each respective sample of said fluid mixtures into a gas chromatograph column of a sorbent material having a greater affinity for said aromatics second component of said fluid mixtures, urging said sample to pass into said column by passing a carrier gas therethrough permitting the balance of said respective fluid mixture to pass through said column in a forward direction while said aromatics second component is retarded therein, sweeping said column of said aromatics therein by reversing the flow direction of said carrier gas therethrough, and at least in part during said sweeping step detecting a physical property of the effluent of the forward end of said column to detect the concentration of said aromatics second fluid component in said respective sample of said fluid mixtures.
Claim 5
Dependent Claim
40 words
The method of claim 2 comprising the further step of heating at least in part during said reacting step (b) said first-named fluid mixture to a temperature in a range at which said reaction of step (b) is thermodynamically favored.
Claim 6
Dependent Claim
74 words
The method of claim 2 wherein said second component of said first-named fluid mixture is distinguishable from said first-named fluid mixture by selective sorbtion of at least one component of said mixture, wherein said reacting step (b) is performed in the presence of a catalyst for converting a substantial portion of said first component into said second component, and wherein said detecting steps (a) and (c) are each performed by the method of chromatography.
Claim 7
Dependent Claim
93 words
The method of claim 2 wherein said first component for detection of said first-named fluid mixture consists essentially of naphthenEs, wherein said reactions of step (b) is performed in the presence of a noble metal catalyst and in the presence of hydrogen for conversion of at least a portion of said naphthenes to aromatics, and wherein said method includes the further step of heating said sample of said first named fluid mixture to a temperature in the range of about 200* to 400* C. at least in part during said reacting step (b).
Claim 8
Dependent Claim
25 words
The method of claim 8 wherein said first fluid mixture consists essentially of fluid components selected from the group consisting of aromatics, naphthenes, and paraffins.
Claim 9
Independent Claim
383 words
An apparatus for detecting a first component of a fluid mixture from a source thereof, said fluid mixture consisting of at least a first component for detection and at least another component said first component having certain physical properties sufficiently similar to those of said other components rendering it difficult to separate or distinguish said first fluid component, comprising: a. means including a chamber packed with a catalyst for subjecting fluid mixture to a chemical reaction converting at least a portion of said first component to a second component distinguishable from said fluid mixture, said chamber having an inlet end and an outlet end, said inlet-end being coupled with said source of said fluid mixture for introduction thereof into said chamber said fluid mixture passing through said outlet end of said chamber after reacting therein; b. a source of a carrier gas coupled with said inlet end of said chamber for carrying said fluid mixture through said chamber; c. heating means operatively coupled with said chamber (a) for heating said fluid mixture at least in part during said reaction thereof in said chamber to a temperature in a range at which said reaction is thermodynamically favored; d. means including a gas chromatograph column and a detector operatively coupled with said outlet end of said chamber (a) for detecting the concentration of said first component in said fluid mixture by detecting said first component converted; e. a source of a reference second fluid mixture having a predetermined concentration therein of said first component, and f. valve means coupled with said source of said reference second fluid mixture and operatively coupled with said inlet of said chamber (a) for periodically introducing into said chamber said reference second fluid mixture for reaction therein and detection of said first component converted of said second fluid mixture enabling periodic calibration of said apparatus in accordance with a proportional relationship relating said detected first component converted of said reference second fluid mixture with said predetermined concentration therein of said first component, said proportional relationship being representative of the relationship between said detected first component converted of said first named fluid mixture and the concentration therein of said first component, said latter concentration being determinable from said calibration-proportional relationship and said detected first component converted of said first-named fluid mixture.
Claim 10
Dependent Claim
215 words
An apparatus according to claim 10 wherein said valve means (f) are further coupled with said source of said first-named fluid mixture and wherein said valve means (f) includes a valve having first and second operative positions said valve when in its first operative position permitting flow therethrough of said first-named fluid mixture for detection of said first component thereof, said valve when in its second operative position permitting flow therethrough of said second fluid mixture for calibration of said apparatus in accordance with said proportional relationship, wherein said reacting means (a) further comprises: a. (g) means including a sample measuring valve coupled with said valve means (f) and operatively coupled with said inlet of said chamber (a,a) for injecting into said chamber periodic samples of substantially constant volume of said first and second fluid mixtures, said sample measuring valve injecting said samples of said first fluid mixture when said valve means (d) is in its second operative position; and a. (h) means including a vaporizer interposed between said sample measuring valve means (a,g) and said chamber (a,a) and coupled with said source of a carrier gas (a,b) for vaporization of said first and second fluid mixtures prior to introduction thereof into said chamber whereby said fluid mixtures are reacted therein in a gaseous state.
Claim 11
Dependent Claim
207 words
An apparatus according to claim 11 wherein said first and second fluid mixtures each include a second component distinguishable from said respective fluid mixtures by gas chromatography, the concentration of said second component in said second fluid mixture being predetermined, wherein said first component at least in part converted of said first and second fluid mixtures is at least in part converted to said second component by said respective reactions thereof, wherein said proportional-calibration relationship relates the concentration of said first component for detection in said first fluid mixture with said detected converted first component converted to said second component of said first and second fluid mixtures and with said predetermined concentrations of said first and second components in said reference second fluid mixture, and wherein said apparatus further comprises: g. means coupled with said source of said first fluid mixture and coupled with said gas chromotograph for injecting into said gas chromatograph vaporized samples unreacted of said first fluid mixture for detection of said second component of said first fluid mixture unreacted, the concentration of said first component in said first fluid mixture being determinable from said detected second component of said first fluid mixture unreacted, said detected first component thereof converted, and said proportional-calibration relationship.
Claim 12
Dependent Claim
205 words
An apparatus according to claim 12 wherein said first component of said first and second fluid mixtures comprises naphthenes, wherein said second component of said first and second fluid mixtures comprises aromatics, wherein said catalyst in said chamber (a,a) comprises a noble metal catalyst for conversion at least in part of said naphthenes to aromatics, wherein said source (a,b) of carrier gas includes hydrogen, wherein said chromatograph column includes a sorbent material therein having a sorbent affinity for aromatics, and wherein said chromatograph column means further includes means including a backflush valve coupled with the inlet and outlet ends of said chromatograph column and coupled with said detector for backflushing said chromatograph column subsequent to each respective injection therein of each of said samples of said first and second fluid mixtures, said chromatograph column being backflushed subsequent to sorbtion therein of at least a portion of said aromatics and passage therethrough of at least a substantial portion of the balance of said respective fluid samples, the backflush flow of said column passing through said detector for detection of the aromatics content of said samples, whereby the concentration of said naphthenes first component in said first fluid mixture is determinable in accordance with said calibration relationship.
Claim 13
Dependent Claim
331 words
The apparatus of claim 13 wherein said chamber (a,a) comprises a reaction chamber of about 5 feet of length of about 3/16-inch diameter steel tubing packed with platinum reforming catalyst having 35 to 80 mesh-particle size, wherein said heating means (a,c) includes a temperature controlled enclosure in which is mounted said reaction chamber, said enclosure including heating means for heating said reaction chamber to a temperature in the range of 200* to 400* C. wherein said chromatograph column comprises a column of about 10 feet of length of about 1/4 -inch diameter steel tubing packed with beta, beta''-thiodipropionitrile deposited on a support of about 60 to 80 mesh-particle size for adsorbtion of said aromatics component and detection thereof, wherein said detector includes means for generating a detector signal the time integral of which is representative of the concentration in said respective samples passed therethrough of said aromatics component, said apparatus of claim 24 further comprising: h. means including a pressure regulator coupled with the outlet end of said chromatograph column for regulating the pressure in said reaction chamber and said chromatograph column in the range of 30 to 60 p.s.i.g.; and i. computing means including integration means coupled with said detector for computing the concentration of said naphthene first component for detection in said first fluid mixture in accordance with said proportional calibration relationship, said relationship being substantially in accordance with the following equation:Y Y1(x2- x1)/(z2- z1) where: Y percent of said naphthene first component for detection in said first fluid mixture, Y1 percent of said naphthene first component in said reference second fluid mixture, x2 percent of said aromatics in said first fluid mixture after said reaction thereof in said chamber, x1 percent of said aromatics in said first fluid mixture prior to said reaction thereof, z2 percent of said aromatics in said reference second fluid mixture after said reaction thereof, and: z1 percent of said aromatics second component in said reference second fluid mixture prior to said reaction thereof.
Claim 14
Dependent Claim
266 words
The apparatus of claim 14 wherein said computing means (i) comprises: ia. manual entry and signal-generating means for entering into said computer the value of said predetermined concentration of said naphthene first component in said reference second fluid mixture and for generating a concentration second signal representative thereof; ib. integration means coupled with said detector for integrating said detector signal and for generating third, fourth, fifth and sixth signals representative of said respective concentrations of said detected aromatics component in said fluid samples passed therethrough, said signals being representative respectively of said quantities: z1, z2, x1, and x2; ic. first difference measuring means coupled with said integration means (ib) for generating a difference seventh signal representative of the difference (z2- z1) between said fourth and third signals; id. second difference measuring means coupled with said integration means (ib) for generating a difference eighth signal representative of the difference (x2- x1) between said sixth and fifth signals; ie. first multiplication means coupled with said second difference measuring means (id) and coupled with said manual entry means (ia) for generating a product ninth signal representative of the product of said concentration second signal and said difference eighth signal; and if. division means including output means coupled with said first multiplication means (ie) and coupled with said first difference measuring means (ic) for generating an output first signal representative of the quotient of said product ninth signal divided by said difference seventh signal, said output first signal corresponding to the concentration of said naphthene first component for detection in said first fluid mixture in accordance with said proportional-calibration relationship.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1974-09-20 | 1975-03-22 | 1975-09-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1978-09-20 | 1979-03-22 | 1979-09-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1982-09-20 | 1983-03-22 | 1983-09-21 | $7700.00 | Window Closed / Lapsed |