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Automated temperature programmed preparative chromatography

Assignee: Phillips Petroleum Co
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Filing: 1977-10-25
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Granted: 1979-05-15
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Expires: 1997-10-25
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Abstract

Abstract An apparatus and method for separating and collecting chromatographic samples in which three separate chromatographic columns are cycled through an elution mode, an elevated temperature back-flush mode, and a cooling back-flush mode in continuous repetition so that at any one time one of the columns is in an elution mode, another of the columns is in elevated temperature back-flush mode, and the remaining column is in cooling back-flush mode.

Inventors

  • 👤 John A. Favre
  • 👤 Lloyd E. Gardner

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 15:25
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/26; G01N30/28; G01N30/30; G01N30/04; G01N30/06; G01N30/12; G01N2030/121; G01N2030/123; G01N30/38; G01N30/40; G01N30/46; G01N30/468; G01N30/80; G01N30/82

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 142 words
An apparatus for separating and collecting chromatographic samples said apparatus comprising: (a) three separate chromatographic columns each provided with means for temperature control; (b) containing lines and valving for supplying and removing samples and flushing gas to each of the columns; (c) means for automatically coordinating temperature and flow through the three columns so that, simultaneously, one column is maintained at a programmed elution temperature while sample gas is passed therethrough, another column is maintained at a temperature elevated above the elution temperature while a stream of flushing gas is passed therethrough, and the remaining column is maintained at a temperature decreasing to elution temperature while another stream of flushing gas is passed therethrough; and (d) means for automatically sequencing temperature control and flow so the each column is cycled through elution flow, heated flush, and decreasing to elution temperature flow seriatim.
Claim 2
Independent Claim 142 words
An apparatus for separating and collecting chromatographic samples said apparatus comprising: (a) three separate chromatographic columns each provided with means for temperature control; (b) containing lines and valving for supplying and removing samples and flushing gas to each of the columns; (c) means for automatically coordinating temperature and flow through the three columns so that, simultaneously, one column is maintained at a programmed elution temperature while sample gas is passed therethrough, another column is maintained at a temperature elevated above the elution temperature while a stream of flushing gas is passed therethrough, and the remaining column is maintained at a temperature decreasing to elution temperature while another stream of flushing gas is passed therethrough; and (d) means for automatically sequencing temperature control and flow so the each column is cycled through elution flow, heated flush, and decreasing to elution temperature flow seriatim.
Claim 3
Dependent Claim 20 words
An apparatus of claim 1 wherein each chromatographic column is in a separate chamber provided with means for temperature control.
Claim 4
Dependent Claim 29 words
An apparatus of claim 1 wherein the means for passing flushing gas directs flow of flushing gas in a direction countercurrent to that in which sample gas is passed.
Claim 5
Independent Claim 106 words
A method for separating and collecting chromatographic samples said method comprising: (a) passing sample through a first column maintained at elution temperature; (b) simultaneously passing a stream of flush gas thorugh a second column maintained at a temperature elevated above elution temperature; (c) simultaneously passing another stream of flush gas through a third column maintained at a temperature decreasing to elution temperature; and (d) sequencing change of flow through said first, second, and third columns so that each column is passed thorugh a sequence of flow patterns in the order of sample elution followed by elevated temperature flush followed by elution temperature flush in continuous repetition.
Claim 6
Independent Claim 106 words
A method for separating and collecting chromatographic samples said method comprising: (a) passing sample through a first column maintained at elution temperature; (b) simultaneously passing a stream of flush gas thorugh a second column maintained at a temperature elevated above elution temperature; (c) simultaneously passing another stream of flush gas through a third column maintained at a temperature decreasing to elution temperature; and (d) sequencing change of flow through said first, second, and third columns so that each column is passed thorugh a sequence of flow patterns in the order of sample elution followed by elevated temperature flush followed by elution temperature flush in continuous repetition.
Claim 7
Dependent Claim 23 words
A method of claim 4 wherein flushing gas is passed through the columns in a direction countercurrent to the flow of sample gas.
Claim 8
Dependent Claim 16 words
A method of claim 4 wherein there is automatic control and sequencing of temperatures and flush.
Claim 9
Dependent Claim 43 words
A method of claim 4 wherein the sample is a gasoline fraction, said elution temperature is in the range of about 100° C. to about 200° C. and said elevated temperature is in the range of about 200° C. to about 300° C.
Claim 10
Dependent Claim 19 words
A method of claim 6 wherein change of flow is sequenced to change about every 5 to 15 minutes.

References Cited (Backward Citations)

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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) 1982-05-14 1982-11-13 1983-05-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1986-05-14 1986-11-13 1987-05-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1990-05-14 1990-11-13 1991-05-15 $7700.00 Window Closed / Lapsed

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