A MICRO GAS CHROMATOGRAPH WITH INTEGRATED
BI-DIRECTIONAL PUMP FOR QUANTITATIVE ANALYSES
Yutao Qin and Yogesh B. Gianchandani
Center for Wireless Integrated MicroSensing and Systems (WIMS
2
)
University of Michigan, Ann Arbor, MI 48109, USA
ABSTRACT
This paper describes a micro gas chromatography
(μGC) system that comprises a Knudsen pump with bi-
directional capability (KP2), a two-stage preconcentrator-
focuser (PCF2) and a separation column. In this valveless
system, the bi-directionality of the pump allows flow
reversal in the multi-stage preconcentrator. The KP2, PCF2,
and separation column are arranged in a 4.3 cm
3
stack, and
used with a commercial flame ionization detector. In
preliminary experiments, the μGC system demonstrated
quantitative separation of benzene, toluene, and xylene
(BTX) in ambient room air.
INTRODUCTION
Typical μGC systems include several components: the
preconcentrator, which accumulates vapor analytes and
provides vapor injection; the column, which separates the
vapor analytes; the gas detector, which quantifies the eluents
(retention peaks) from the column; and the gas pump, which
provides flow [1-3]. In the simplest architectures, the
preconcentrator, column, detector, and pump are connected
in series, and operated with unidirectional flow [4-5]. In
more complex architectures, valves are used to create
opposite flow directions (bi-directional flow) in the
preconcentrator during sampling and separation; examples
appear in [6-8].
While bi-directional flow is potentially beneficial for a
single-stage preconcentrator, it is essential for a multi-stage
(or multi-bed) one. A multi-stage preconcentrator has
different sorbents packed in its stages that are connected in
series (Fig. 1). Weaker stages – those packed with lower
surface-area sorbents – are located upstream in the sampling
flow and are intended to trap vapor analytes with lower
volatility. Stronger stages – those packed with higher
surface-area sorbents – are located downstream in the
sampling flow, and are intended to trap vapor analytes with
higher volatility that pass through weaker stages [9]. The
vapor sample must flow from the weaker stages to the
stronger stages to permit upstream capture of low volatility
analytes during the sampling phase. In the analytical
separation phase, the flow is reversed, allowing the low
volatility sample to enter the separation column together
with the high volatility sample that was captured deeper
within the preconcentrator. In conventional systems, the
flow reversal is accomplished by valves [6-8].
This effort explores a valveless μGC architecture,
which is comprised of a bi-directional Knudsen pump
(KP2), a two-stage preconcentrator (PCF2), and a separation
column. During vapor sampling, vapor analytes enter the
μGC system through the separation column and settle into
the PCF2 (Fig. 1). During analytical separation, the flow is
reversed by the KP2; the sampled vapor analytes are then
thermally desorbed from the PCF2 and separated in the
column. A commercial flame ionization detector (FID) is
used as the detector for accurate quantification of the bi-
directional operation. In the future, a micro gas detector can
be integrated for realizing a complete, bi-directional μGC
system.
DESIGN
Bi-Directional Knudsen Pump (KP2)
Knudsen pumps operate by thermal transpiration [10].
High reliability and simple configuration make these pumps
attractive for integration with µGC systems [5, 11]. One
example of a Knudsen pump implementation utilizes
nanoporous mixed cellulose ester (MCE) membrane(s)
(thickness ≈105 μm, pore diameter ≈25 nm, porosity ≈70%,
Millipore, MA) [12]. In the presence of a temperature
gradient, thermal transpiration flow is generated from the
cold side to the hot side of the membranes. A previously
reported bi-directional Knudsen pump used thermoelectric
elements to provide reversible temperature gradients and gas
flow [13]. In this effort, however, the bi-directional
Knudsen pump is implemented simply by integrating
resistive heaters on both sides of the MCE membranes.
During operation, one of the sides is heated while the other
is cooled (by a heat sink or natural convection), providing a
temperature gradient.
The KP2 consists of four glass dice (Die 1a, 1b, 2a, and
2b, thickness =500 μm) sandwiching a stack of four MCE
membranes (Fig. 2). Side-A of the KP2 consists of Die 1a
Fig. 1: Concept of multi-stage preconcentrator and the bi-
directional operation of the μGC system in this effort.
978-1-4799-3509-3/14/$31.00 ©2014 IEEE 294 MEMS 2014, San Francisco, CA, USA, January 26 - 30, 2014