Gas separation: processes – Chromatography – With heating or cooling
Reexamination Certificate
2002-01-31
2003-12-23
Spitzer, Robert H. (Department: 1724)
Gas separation: processes
Chromatography
With heating or cooling
C073S023360, C073S023390, C096S102000, C096S105000, C096S107000
Reexamination Certificate
active
06666907
ABSTRACT:
BACKGROUND OF THE INVENTION
The present invention relates generally to chemical separations in microanalytical systems and, more particularly, to temperature programming of a microfabricated gas chromatography column for efficient separation of gas-phase analytes.
Portable, handheld microanalytical systems, which have been termed “chemical laboratories on a chip,” are being developed to enable the rapid and sensitive detection of particular chemicals, including pollutants, high explosives, and chemical warfare agents. These microanalytical systems should provide a high chemical selectivity to discriminate against potential background interferents and the ability to perform the chemical analysis on a short time scale. In addition, low electrical power consumption is needed for prolonged field use. See, e.g., Frye-Mason et al., “Hand-Held Miniature Chemical Analysis System (&mgr;ChemLab) for Detection of Trace Concentrations of Gas Phase Analytes,”
Micro Total Analysis Systems
2000, 229 (2000).
Current gas-phase microanalytical systems are based on gas chromatography (GC). Gas chromatography relies upon the chemical equilibria of analytes between a mobile phase and a stationary phase in a GC column to bring about a temporal separation of analytes in a gas mixture. Chemical equilibria and, therefore, column retention times are strongly influenced by column temperature. Thus, column temperature must be precisely controlled to obtain accurate separations.
The goal of a GC analysis is normally to obtain a separation with the required accuracy in the minimum time. Isothermal operation of the GC column can have drawbacks for achieving this goal with certain gas mixtures. If the selected isothermal temperature is too low, early-eluted peaks will be closely spaced whereas more strongly retained analytes will have broad and low-lying peaks and consequent poor detectability. Conversely, the more strongly retained analytes will elute faster at a higher isothermal column temperature, but at the expense of poorer separation and loss of resolution for the early eluting analytes.
This general elution problem may be solved by temperature programming of the column. With temperature programming, analysis time can be reduced and the overall detectability of components can be improved. For example, for a given column it is possible to analyze gas mixtures with a broader volatility range in a shorter analysis time with temperature programming. For most analytes, the baseline resolution and peak widths are also improved. In general, temperature programming can comprise a series of changes in the column temperature that can include isothermal and controlled temperature rise segments. As an example of temperature programming, consider temperature ramping. Temperature ramping comprises monotonically increasing the temperature as the gas mixture is passed through the column. Higher volatility analytes in the mixture, which without temperature ramping pass through the column the earliest, still are the first to arrive at the column exit. Temperature ramping only tends to modestly improve the peak widths of these early eluting analytes and enhances baseline resolution somewhat. This is mainly due to the fact that these faster eluting analytes pass through the column before the initial temperature is appreciably increased. On the other hand, less volatile analytes, which in the absence of ramping tend to elute slowly with relatively broad and low-lying peaks, elute more quickly with temperature ramping and are generally improved from the standpoint of baseline resolution and peak width. As a result, analysis time can be improved relative to a low temperature, isothermal elution while retaining resolution.
In conventional chromatography, an oven enclosing the GC column is used to effect the temperature program. This process is energy intensive, requiring hundreds of watts of power, and is capable of providing only modest ramp rates of about 25° C./min. These characteristics are adequate for laboratory applications where power is not that limited, and long, 30 meter columns can be used to separate difficult mixtures without the need for faster ramp rates. However, for portable applications, this level of power consumption is unacceptable. Further, given the necessarily shorter length of portable GC columns relative to laboratory instruments, more rapid temperature ramping can compensate for the loss of resolution due to fewer theoretical plates in the portable GC column. Thus, there exists a need for temperature programming of microfabricated GC columns suitable for a portable, energy-efficient microanalytical system.
The present invention solves the need for a temperature programmable microfabricated GC column through the integration of a resistive heating element and temperature sensing on microfabricated GC column. Additionally, means are provided to thermally isolate the heated-column from its surroundings. The thermal isolation reduces power losses from the heated zone and reduces column heat capacity, thereby improving the thermal time response and power consumption, both important factors for portable GC applications. The present invention permits rapid, low-power and sensitive temperature programming of the microfabricated GC column and temperature ramp rates that are an order of magnitude faster than conventional GC columns, thereby enabling more efficient chemical separations.
SUMMARY OF THE INVENTION
The present invention comprises a temperature programmable microfabricated gas chromatography column comprising a substrate, a channel etched in the substrate to separate chemical analytes in a gas mixture, at least one lid disposed on a channel-side of the substrate to seal the channel, and at least one resistive heating element disposed on a least one surface of the substrate to heat the column during the separation. The temperature programmable microfabricated gas chromatography column can further comprise a control board for electrical control of the resistive heating element and fluidic control of the column, means for electrically connecting the control board to the resistive heating element, means for fluidically connecting the control board to the channel, and means for thermal isolation of control board from the substrate.
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Men
Frye-Mason Gregory C.
Manginell Ronald P.
Bieg Kevin W.
Sandia Corporation
Spitzer Robert H.
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