# US 2019/0170708 A1 · Method and system for reducing the effects of column bleed carryover > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2019/0170708 A1 - Document ID: US20190170708A1 - Status: Published application - Kind: A1 - Application number: 16/314,415 - Filed: 2016-06-29 - Published: 2019-06-06 - Earliest claimed: 2016-06-29 - Assignees: Agilent Technologies, Inc. - Applicants: Agilent Technologies, Inc. - Inventors: Paul C. Dryden; Sammye Elizabeth Traudt; Robert C. Henderson - Web page: https://patentgrep.com/patent/US20190170708A1 ## CPC - G01N 30/30: of temperature - G01N 30/16: Injection (G01N30/24 takes precedence) - G01N 30/32: of pressure or speed (G01N30/36 takes precedence) - G01N 30/54: Temperature - G01N 30/8658: {Optimising operation parameters} - G01N 2030/025: {Gas chromatography} - G01N 2030/167: {on-column injection} - G01N 2030/3076: {using specially adapted T(t) profile} - G01N 2030/324: {speed, flow rate} - 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) ## Abstract In gas chromatography (GC), a sample is introduced into a flow of carrier gas and the mixture is driven through a heated GC column to acquire chromatographic data from the sample. During this time, the column is heated from an initial temperature to a final temperature. Subsequently, the column is cooled according to a cooling program. The cooling program may include a first cooling ramp, a subsequent isothermal hold, and a subsequent second cooling ramp. Alternatively, while the column is cooled down the flow of carrier gas through the column may be slowed down or ceased for a period of time, after which the flow of carrier gas through the column may be resumed at the original flow rate in preparation for processing another sample. Controlling column temperature and/or flow in this manner may be effective for reducing column bleed carryover and/or the effects thereof. ## Claims ### Claim 1 A method for performing gas chromatography (GC) on a sample, the method comprising: flowing a carrier gas through a GC column; during a sample run time, heating the GC column according to a heating program, the heating program comprising increasing a column temperature of the GC column from an initial temperature to a final temperature; during the sample run time, injecting the sample into the flowing carrier gas to produce a mixture of the sample and the carrier gas, and flowing the mixture through the GC column; and after the sample run time, cooling the GC column according to a cooling program, the cooling program comprising: decreasing the column temperature from the final temperature to a dwell temperature; holding the column temperature at the dwell temperature for an isothermal dwell time; and after the isothermal dwell time, decreasing the column temperature from the dwell temperature to the initial temperature. ### Claim 2 (depends on 1) The method of claim 1, wherein the dwell temperature is a temperature cool enough to substantially avoid decomposition of a stationary phase of the GC column phase and warm enough to promote flushing away of decomposition products existing in the GC column prior to the sample run time. ### Claim 3 (depends on 1) The method of claim 1, wherein the dwell temperature is in a range from about 20° C. to about 100° C. below the final temperature. ### Claim 4 (depends on 1) The method of claim 1, wherein the isothermal dwell time is a period of time effective to allow decomposition products existing in the GC column prior to the sample run time to be flushed from the GC column. ### Claim 5 (depends on 1) The method of claim 1, comprising defining a flushing time as the sum of a duration over which decreasing the column temperature from the final temperature to the dwell temperature occurs and the isothermal dwell time, wherein the flushing time is selected from the group consisting of: a period of time in a range from about 1 time to about 4 times a void time of the GC column; and a period of time in a range of about 1 minute to 5 minutes. ### Claim 6 (depends on 1) The method of claim 1, wherein decreasing the column temperature from the final temperature to the dwell temperature, or decreasing the column temperature from the dwell temperature to the initial temperature, or both of the foregoing, is done at a cooling rate in a range from 100° C./min to 1000° C./min. ### Claim 7 (depends on 1) The method of claim 1, wherein decreasing the column temperature from the final temperature to the dwell temperature is done at a first cooling rate, decreasing the column temperature from the dwell temperature to the initial temperature is done at a second cooling rate, and the first cooling rate is greater than the second cooling rate. ### Claim 8 (depends on 1) The method of claim 1, comprising, at or after a start time of holding the column temperature at the dwell temperature for the isothermal dwell time, increasing a column flow rate from an initial flow rate to an elevated flow rate, and holding the column flow rate at the elevated flow rate for a flow rate hold time spanning at least a portion of the isothermal dwell time. ### Claim 9 (depends on 8) The method of claim 8, wherein increasing the column flow rate comprises increasing a column inlet pressure. ### Claim 10 (depends on 1) The method of claim 1, comprising, during the sample run time, flowing the mixture from the GC column to a detector to acquire chromatographic data from the sample. ### Claim 11 (depends on 1) The method of claim 1, wherein cooling the GC column according to the cooling program is performed after analytes of interest have eluted from the column. ### Claim 12 A gas chromatography (GC) system, comprising: a GC column; a carrier gas source configured for flowing a mixture of a sample and a carrier gas through the GC column; a heating device configured for heating the GC column; and a controller configured for: controlling the carrier gas source to flow the mixture through the GC column during a sample run time; controlling the heating device to heat the GC column during the sample run time according to a heating program, the heating program comprising increasing a column temperature of the GC column from an initial temperature to a final temperature; and controlling the heating device to cool the GC column after the sample run time according to a cooling program, the cooling program comprising: decreasing the column temperature from the final temperature to a dwell temperature; holding the column temperature at the dwell temperature for an isothermal dwell time; and after the isothermal dwell time, decreasing the column temperature from the dwell temperature to the initial temperature. ### Claim 13 (depends on 12) The GC system of claim 12, wherein the controller is configured for maintaining the dwell temperature in a range from about 20° C. to about 100° C. below the final temperature. ### Claim 14 (depends on 12) The GC system of claim 12, wherein a flushing time is defined as the sum of a duration over which decreasing the column temperature from the final temperature to the dwell temperature occurs and the isothermal dwell time, wherein the controller is configured for controlling the heating device such that the flushing time is selected from the group consisting of: a period of time in a range from about 1 time to about 4 times a void time of the GC column; and a period of time in a range of about 1 minute to 5 minutes. ### Claim 15 (depends on 12) The GC system of claim 12, wherein the controller is configured for controlling the heating device such that decreasing the column temperature from the final temperature to the dwell temperature, or decreasing the column temperature from the dwell temperature to the initial temperature, or both of the foregoing, is done at a cooling rate in a range from 100° C./min to 1000° C./min. ### Claim 16 (depends on 12) The GC system of claim 12, wherein the controller is configured for controlling the heating device such that decreasing the column temperature from the final temperature to the dwell temperature is done at a first cooling rate, decreasing the column temperature from the dwell temperature to the initial temperature is done at a second cooling rate, and the first cooling rate is greater than the second cooling rate. ### Claim 17 (depends on 12) The GC system of claim 12, wherein the controller is configured for: at or after a start time of holding the column temperature at the dwell temperature for the isothermal dwell time, increasing a column flow rate from an initial flow rate to an elevated flow rate, and holding the flow rate at the elevated flow rate for a flow rate hold time spanning at least a portion of the isothermal dwell time. ### Claim 18 (depends on 12) The GC system of claim 12, comprising a cooling device configured for actively cooling the GC column, wherein the controller is configured for controlling the cooling device to cool the GC column after the sample run time according to the cooling program. ### Claim 19 A method for performing gas chromatography (GC) on a sample, the method comprising: flowing a carrier gas through a GC column; during a sample run time, heating the GC column to a predetermined temperature or according to a predetermined temperature profile; during the sample run time, injecting the sample into the flowing carrier gas to produce a mixture of the sample and the carrier gas, and flowing the mixture through the GC column; after the sample run time, cooling the GC column during a cooling time; and during at least an initial portion of the cooling time, reducing or ceasing the flowing of the carrier gas through the GC column. ### Claim 20 (depends on 1) A non-transitory computer-readable medium with instructions stored thereon, that when executed by a processor, control or perform cooling the GC column according to the method of claim 1.