Measuring and testing – Gas analysis – Gas chromatography
Reexamination Certificate
2001-06-05
2003-09-02
Lefkowitz, Edward (Department: 2856)
Measuring and testing
Gas analysis
Gas chromatography
C073S863720, C137S884000
Reexamination Certificate
active
06612153
ABSTRACT:
FIELD OF INVENTION
The present invention relates generally to miniaturized planar device for liquid and gas phase analysis. More specifically, the invention relates to a planar manifold that integrates heated inlets with unheated pneumatics on the same plate.
BACKGROUND OF THE INVENTION
A gas chromatograph (GC) is an analytical instrument that takes a gaseous sample (or converts a sample to the gaseous state if necessary), and separates the sample into individual compounds, allowing the identification and quantification of those compounds. The principal components of a typical gas chromatograph are the following: an injector that converts sample components into gases (if necessary) and moves a representative sample of the mixture onto the head of a separation column in a narrow band; a separation column that separates the sample mixture into its individual components as these components are swept through the column by an inert carrier gas, the separation being based on differential interactions between the components of the sample mixture and an immobilized liquid or solid material within the column; a detector that detects and measures components as they exit the separation column; and a data display.
Typical modern GC instruments are configured with a heated-block “flash evaporator” type injector, a long capillary tube column, an oven housing the column to maintain and to change the column's temperature in a predictable and reproducible fashion, a flame ionization detector (or other type of detector), and a computer with dedicated hardware/software to process the data collected. Conventional GC units are typically about the size of a large microwave oven (50-100 kg), require 2 to 3 kilowatts of power and considerable air conditioning.
Micro GCs are portable GC systems that are light, rugged and fast. Micro GCs use only utilities (compressed gas and electricity) that are readily available in the field. The micro GCs, smaller than a briefcase, have been widely used not only in field applications, such as custody transfer, well logging, environmental screening, and storage tank analysis, but also in laboratories because micro GCs require minimal laboratory space and operate at high speed with minimal consumption of utilities (compressed gases, air conditioning, etc.).
An important part of a GC system is the accurate control of fluid flow, which is typically achieved with an extensive and complex array of channels, tubing, fittings and the like in a conventional GC. U.S. Pat. No. 5,686,657, herein incorporated by reference, discloses a method to reduce external connections between fluid-handling devices by use of a single planar manifold for the provision of a plurality of flow paths. The fluid-handling devices that connect to the planar manifold are preferably constructed to be surface-mounted, which has been found to offer reliable, fluid-tight connection without the complexity and difficulty of conventional pneumatic connections. The number and complexity of external connections, which would otherwise undesirably increase the volume of the flow system, are also decreased. Another advantage is that the reliability of the pneumatic connections is improved.
A further advantage of the planar manifold technology is that multiple fluid-handling functional devices may be coordinated and assembled in a small volume. Multiple pneumatic channels can be integrated in a planar manifold, which is itself quite compact and amenable to construction in a variety of shapes and configurations. For example, it is contemplated that a planar manifold may be constructed in an irregular shape, such as a curved, bent, or multiple-angled configuration, so as to conform to an irregularly-shaped, compact volume.
A diffusion bonding method is one of the preferred methods to manufacture planar manifolds. In the diffusion bonding method, bonding members to be bonded to each other are held in close contact with each other, and pressed to a degree so that the bonding members are bonded by the diffusion of atoms which takes place in the interface between the bonded surfaces. Since the bonding members are actually “melted” into each other under the bonding conditions, diffusion bonding provides satisfactory bonding strength, air-tightness, and pressure resistance that are required in a pressured fluid-handling system.
Diffusion bonded planar manifolds have been used to perform gas supply functions that relate to injector inlets or detectors in conventional GCs, such as the Agilent 6890 Plus GC system.
FIG. 1
shows a block diagram of a prior art GC unit
10
. This typical GC unit
10
comprises a computer
12
, a controller
14
, an injector inlet
16
, a detector
18
, a column
20
, an oven
22
, a column heater
28
, and a plurality of planar manifolds
24
and
26
.
In order to perform a chromatographic separation of a given sample compound, a sample is injected with a pressurized carrier gas by means of the injector inlet
16
. The carrier gas supplied to inlet
16
is provided from a source
16
A through one or more inlet planar manifold(s)
24
, each of which serves in part to control and redirect a plurality of gas flows. The column
20
is positioned within the oven
22
which has an operating temperature of between room temperature and about 450° C. The carrier gas/sample combination passing through column
20
is exposed to a temperature profile resulting in part from the operation of the column heater
28
within oven
22
. During this profile of changing temperatures, the sample will separate into its components primarily due to differences in the interaction of each component with the column
20
at a given temperature. As the separated components exit the column
20
, the components are detected by the detector
18
which requires a plurality of detector gasses of appropriate types, such as air, hydrogen, and make-up gas. The detector gases are provided from respective sources
18
A through one or more detector planar manifold(s)
26
. The inlet planar manifolds
24
and detector planar manifolds
26
are placed in a GC manifold carrier
30
. Suitable fluid-handling devices, such as fittings, regulators, valves, sensors, and the like in the planar manifolds
24
and
26
may be passive (such as a termination fitting) or active and hence operated under the control of the computer
12
by way of control signals provided the controller
14
.
To avoid a “cold spot” or “condensing point”, the injector inlet
16
and detector
18
are both heated in their respective heated zones
17
and
19
. Since the various valves and electronic pressure controls (EPC) in the planar manifolds
24
and
26
are usually operated at room temperature, the GC manifold carrier
30
is located outside the oven
22
and is connected to the inlet
16
and the detectors
18
by stainless steel tubing
32
. Furthermore, all prior art designs use separated planar manifolds for injector inlet and detector gas supplies.
Up until now, micro GCs have not used diffusion bonded planar manifold technology. Instead, micro GCs use discrete stainless steel tubing, machined manifold blocks, o-ring seals, and press fit tapered unions with UV-glue to integrate the gas supply pneumatics and injector device together. Micro-GCs are currently designed to use iso-thermal ovens, and operate over a narrower temperature range of between room temperature to about 120° C.
SUMMARY OF THE INVENTION
Disclosed is a diffusion bonded planar manifold integrating a variety of fluid handling devices that require different operating temperatures onto a single plate. The diffusion bonded planar manifold comprises a high temperature zone for devices requiring high operating temperatures, a low temperature zone for devices requiring lower operating temperatures, and an insulating zone to separate the high temperature zone from the low temperature zone. The insulating zone is designed with such a geometry that heat transfer between the high temperature zone and the low temperature zone is minimized while the mechanical rigidity of the diffusion bonded pla
Loux Alan D.
White Richard P.
Cygan Michael
Lefkowitz Edward
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