Patent US3616273A successfully refreshed from Google Patents.
US3616273A
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Nitrogen determination and apparatus therefor
Assignee: Standard Oil Co
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Filing: 1968-04-01
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Granted: 1971-10-26
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Expires: 1988-04-01
Abstract
Abstract A method and apparatus for quantitatively determining the nitrogen content of organic materials, especially those organic materials having boiling points in excess of about 450* F. The method involves hydrocracking the organic material, hydrogenating the nitrogen to ammonia, and measuring the quantity of ammonia present, which may then be related to the original nitrogen composition.
Inventors
- 👤 Itsumi Jack Oita
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 20:55
CPC Classifications
G; G01; G01N; G01N31/00; G01N31/002; Y; Y10; Y10T; Y10T436/00; Y10T436/11; Y10T436/115831; Y10T436/116664; Y10T436/17; Y10T436/176152
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
16 words
The method of claim 1 wherein said hydrocracking catalyst comprises rhodium on a molecular sieve base.
Claim 2
Dependent Claim
145 words
introducing the encapsulated organic material into the vaporizing zone; b. passing effluent from said vaporizing zone which includes vaporized organic material and humidified hydrogen through a hydrocracking zone, said hydrocracking zone including a hydrocracking catalyst, at a temperature in the range of between about 1,400* F. and about 1,440* F.; c. passing effluent from said hydrocracking zone through a bed of nickel granules at a temperature in the range of between about 1,400* F. and about 14402 F.; d. contacting effluent from said bed of nickel granules with a nickel-on-magnesia catalyst at a temperature in the range of between about 680* F. and about 715* F., to convert the nitrogen in said organic material to ammonia; and e. coulometrically titrating the ammonia produced in step (d), the amount of titrant required for said titration being a measure of the nitrogen content in said organic material.
Claim 3
Dependent Claim
26 words
a hydrocracking zone including a hydrocracking catalyst bed and means for maintaining said hydrocracking catalyst bed at a temperature between about 1,400F. and 1,440* F; and
Claim 4
Dependent Claim
141 words
a plug having a well, said plug being rotatably mounted within said passageway, said well being in registration with the passage of said conduit so that as said plug is rotated within said bore, the well alternatively communicates with the upper end of said conduit and the lower end of said conduit; c. analyzing means for quantitatively detecting the presence of ammonia, said analyzing means in fluid communication with said reactor wherein said organic material passes sequentially: d. through said vaporizing zone to insure that said organic material is in the vapor state; e. through said hydrocracking zone to convert said organic material to lower molecular weight components; f. through said hydrogenation zone to convert any nitrogen present to ammonia; and wherein effluent from said hydrogenation zone is passed to said analyzing means to determine the amount of ammonia present therein.
Claim 5
Dependent Claim
26 words
a hydrocracking zone including a hydrocracking catalyst bed and means for maintaining said hydrocracking catalyst bed at a temperature between about 1,400* F. and 1440* F.;
Claim 6
Dependent Claim
125 words
a stopcock mounted for rotation within said hole in said tube, said stopcock at all times preventing flow through the passageway in said tube, said stopcock having a flow passage, one end of which is sealed; c. analyzing means for quantitatively detecting the presence of ammonia, said analyzing means in fluid communication with said reactor wherein said organic material passes sequentially; d. through said vaporizing zone to insure that said organic material is in the vapor state; e. through said hydrocracking zone to convert said organic material to lower molecular weight components; f. through said hydrogenation zone to convert any nitrogen present to ammonia; and wherein effluent from said hydrogenation zone is passed to said analyzing means to determine the amount of ammonia present therein.
Claim 7
Dependent Claim
34 words
a hydrogenation zone containing a nickel-on-magnesia hydrogenation catalyst bed and means for maintaining said hydrogenation catalyst bed at a temperature between about 680* F. and 715* F.; b. inlet means to said reactor comprising:
Claim 8
Dependent Claim
35 words
a hydrogenation zone containing a nickel-on-magnesia hydrogenation catalyst bed and means for maintaining said hydrogenation catalyst bed at a temperature between about 680* F. and 715* F.; and b. inlet means to said reactor comprising:
Claim 9
Dependent Claim
14 words
The method of claim 2 wherein said hydrocracking catalyst comprises about 0.6 percent rhodium.
Claim 10
Dependent Claim
15 words
The method of claim 1 wherein said hydrocracking catalyst comprises rhodium on a silica-alumina base.
Claim 11
Dependent Claim
14 words
The method of claim 4 wherein said hydrocracking catalyst includes about 0.6 percent rhodium.
Claim 12
Dependent Claim
22 words
The method of claim 1 wherein said organic material is mixed with hydrogen gas prior to being passed through said hydrocracking zone.
Claim 13
Dependent Claim
17 words
The method of claim 6 wherein said hydrogen is humidified to inhibit coking of the hydrocracking catalyst.
Claim 14
Independent Claim
177 words
A method for automatically determining the nitrogen content of an organic material comprising: a. Passing said organic material through a vaporizing zone in the presence of humidified hydrogen, wherein said organic material is converted to a vapor phase; b. Passing the effluent from said vaporizing zone which includes vaporizing organic material and humidified hydrogen through a hydrocracking zone, said hydrocracking zone including a hydrocracking catalyst, at a temperature in the range of between about 1,400* F. and about 1,440* F.; c. Passing the effluent from said hydrocracking zone through a bed of nickel granules at a temperature in the range of between about 1,400* F. and about 1,440* F.; d. Contacting the effluent from said bed of nickel granules with a nickel-on-magnesia catalyst at a temperature in the range of between about 680* F. and about 715* F., to convert the nitrogen in said organic material to ammonia; and e. Coulometrically titrating the ammonia produced in step (d), the amount of titrant required for said titration being a measure of the nitrogen content in said organic material.
Claim 15
Dependent Claim
18 words
The method of claim 8 wherein said hydrocracking catalyst comprises 0.6 percent rhodium on a molecular sieve base.
Claim 16
Dependent Claim
17 words
The method of claim 8 wherein said hydrocracking catalyst comprises 0.6 percent rhodium on a silica-alumina base.
Claim 17
Independent Claim
177 words
An apparatus for determining the nitrogen content of an organic material comprising: a. A reactor including in series: i. a vaporizing zone including a heating means for vaporizing said organic material; ii. a hydrocracking zone including a hydrocracking catalyst bed and means for maintaining said hydrocracking catalyst bed at a temperature between about 1,400* F. and 1,440* F; and iii. a hydrogenation zone containing a nickel-on-magnesia hydrogenation catalyst bed and means for maintaining said hydrogenation catalyst bed at a temperature between about 680* F. and 715* F.; and b. Analyzing means for quantitatively detecting the presence of ammonia, said analyzing means in fluid communication with said reactor wherein said organic material passes sequentially: c. Through said vaporizing zone to insure that said organic material is in the vapor state; d. Through said hydrocracking zone to convert said organic material to lower molecular weight components; e. Through said hydrogenation zone to convert any nitrogen present to ammonia; and wherein effluent from said hydrogenation zone is passed to said analyzing means to determine the amount of ammonia present therein.
Claim 18
Dependent Claim
16 words
The apparatus of claim 11 wherein said supply means further includes means for humidifying said hydrogen.
Claim 19
Dependent Claim
32 words
The apparatus of claim 12 wherein said supply means further includes a temperature control means whereby said humidified hydrogen may be supplied to the reactor at a temperature of about 200* F.
Claim 20
Dependent Claim
40 words
The apparatus of claim 11 wherein said analyzing means is a coulometric titrator, wherein said hydrocracking catalyst comprises 0.6 percent rhodium on a molecular sieve base, and wherein said hydrocracking zone further includes at least one bed comprising nickel granules.
Claim 21
Dependent Claim
37 words
The apparatus of claim 14 wherein said analyzing means is a coulometric titrator, wherein said hydrocracking catalyst comprises 0.6 percent rhodium on silica-alumina, and wherein said hydrocracking zone further includes at least one bed comprising nickel granules.
Claim 22
Dependent Claim
36 words
The apparatus of claim 11 further including a hydrogen supply means in fluid communication with said reactor and adapted to supply hydrogen to said reactor at a point within said reactor prior to said hydrocracking zone.
Claim 23
Independent Claim
32 words
A method for automatically determining the nitrogen content of an organic material comprising: a. introducing said organic material into a vaporizing zone in the presence of humidified hydrogen by the steps of
Claim 24
Dependent Claim
11 words
The method of claim 17 wherein the encapsulating material is tin.
Claim 25
Independent Claim
18 words
An apparatus for determining the nitrogen content of an organic material comprising: a. a reactor including in series:
Claim 26
Independent Claim
18 words
An apparatus for determining the nitrogen content of an organic material comprising; a. a reactor including in series:
References Cited (Backward Citations)
No citation records indexed.
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1974-10-25 | 1975-04-26 | 1975-10-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1978-10-25 | 1979-04-26 | 1979-10-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1982-10-25 | 1983-04-26 | 1983-10-26 | $7700.00 | Window Closed / Lapsed |