Information
-
Patent Grant
-
6789330
-
Patent Number
6,789,330
-
Date Filed
Thursday, December 21, 200024 years ago
-
Date Issued
Tuesday, September 14, 200420 years ago
-
Inventors
-
Original Assignees
-
Examiners
Agents
- Sterne, Kessler, Goldstein & Fox PLLC
-
CPC
-
US Classifications
Field of Search
US
- 034 343
- 034 362
- 034 363
- 034 364
- 034 380
- 034 413
- 034 443
- 034 470
- 034 477
- 034 487
- 034 493
- 422 108
- 422 171
- 422 190
- 422 109
-
International Classifications
-
Abstract
An apparatus and method for quickly drying solutions in one or more arrays of vessels includes a manifold that receives gas and a base plate that receives the one or more arrays of vessels. The manifold includes one or more hollow tubes that direct the gas into the vessels, where the gas evaporates the solutions. A variety of types of hollow tubes are disclosed. In an exemplary embodiment, the gas is filtered, pressurized and/or heated. In an exemplary embodiment, the solutions are heated. The base plate is hingeably coupled to the manifold so that the base plate has an open position and a closed position. The open position permits users to place and remove the vessels that contain solutions to be dried. In the closed position, the base plate and the manifold are in sealing engagement with one another, wherein the one or more of the hollow tubes extend into the vessels. A unique hinging system is disclosed that couples one or more base plates to a base so that, when the base plate is in the open position, the base plate is substantially horizontal. When the base plate is in the closed position, it is tilted at an angle so that the vessels are tilted at the angle, providing the solutions to be dried with a greater surface area. A variety of optional vapor recovery systems are disclosed. A variety of open loop and closed loop electrical control systems are disclosed.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an apparatus and method for drying solutions containing macromolecules.
2. Background Art
Solutions, such as those used for deoxyribonucleic acid (DNA) synthesis, are often dried for long-term storage. These dried solutions can be reconstituted for use when needed. This technique is particularly useful in areas in which refrigerated storage is prohibitively expensive or unavailable. In these areas, room temperature storage of dried solutions is the only means available to store and use the necessary solutions.
Conventional devices for drying solutions include vacuum and centrifugal force systems, such as those available from Savant Instruments, Inc., of Holbrook, N.Y. These devices use a vacuum to increase the rate of evaporation. A vacuum, however, can cause foaming and bumping, resulting in sample loss and contamination of other samples. Moreover, vacuum pumps can be damaged by the solutions being dried and thus require vapor traps. Centrifugal force, generated by spinning the samples, may reduce foaming and bumping. However, mechanisms for spinning the samples include rotors and motors that have to be carefully balanced. Balancing includes loading samples to be dried in prescribed manners. Failure to maintain proper balance can lead to oscillating vibrations that can cause catastrophic failure of rotors and motors. Conventional drying systems can take several hours to dry a set of solutions.
What is needed is a reliable, low maintenance, apparatus and method for quickly drying solutions in large arrays of vessels.
BRIEF SUMMARY OF THE INVENTION
The present invention is an apparatus and method for quickly drying solutions in large arrays of vessels. The apparatus includes a dryer manifold that holds large arrays of vessels which contain solutions to be dried. The solutions to be dried can include macro-molecules such as ribonucleic acid (RNA), DNA, oligonucleotides, proteins, lipids, carbohydrates, polypeptides, cells, chemical compounds and combinations thereof. Gas, which can be inert gas, air, oxygen, nitrogen, or any other gas or mixture of gasses that are suitable for drying solutions, is provided to the dryer manifold, which directs the gas into the arrays of vessels. Preferably, the gas is pressurized. More preferably, the gas is pressurized and heated. More preferably still, the gas is pressurized, heated and filtered. Preferably, the solutions to be dried are heated. The combination of heating the solutions and directing heated gas over the solutions, quickly evaporates the solutions to be dried. Exhaust vapors are removed from the vessels and is optionally captured by a vapor recovery system.
In an exemplary embodiment, the dryer manifold includes a manifold that receives gas and a base plate that receives the array of vessels that contain solutions to be dried. In an exemplary embodiment, the manifold includes a nozzle plate which has an array of passages therethrough. A hollow tube extends downwardly from each of the passages and towards the base plate. A baffle within the manifold guides the gas through the nozzle plate passages and through the hollow tubes. The hollow tubes direct the gas into the vessels, where the gas evaporates the solutions. Preferably, the hollow tubes extend into the vessels.
Preferably the dryer manifold heats the solutions to be dried. For example, the base plate can be heated. In an exemplary embodiment, the base plate receives one or more removable vessel tray that hold a plurality of vessels. The heated base plate heats the solutions in the vessel trays.
The present invention can employ a variety of types of downwardly extending hollow tubes to provide the gas into the vessels. In an exemplary embodiment, one or more of the downwardly extending hollow tubes include a substantially downwardly-facing opening that directs the gas substantially directly at a surface of a solution in a vessel. In another exemplary embodiment, one or more of the downwardly extending hollow tubes include one or more substantially horizontally-facing openings that direct the gas substantially horizontal to a surface of a solution in a vessel. In another exemplary embodiment, the present invention employs a combination of substantially downwardly-facing openings and substantially horizontally-facing openings.
The present invention can utilize an inlet filter, such as a high extraction particulate air (HEPA) filter, to filter the gas that is provided to the dryer manifold. An inlet fan can be utilized to pressurize the gas and an inlet heater can be utilized to heat the gas. An exhaust fan can be utilized to draw exhaust vapors from the dryer manifold.
In an exemplary embodiment, the base plate is hingedly coupled to the manifold so that the base plate has an open position and a closed position. The open position permits users to place and remove vessels in the dryer manifold. In the closed position, the base plate and the manifold are in sealing engagement with one another. Preferably, when in the closed position, the downwardly extending tubes extend into the vessels without contacting the vessels and contacting the solutions in the vessels.
In an exemplary embodiment, when the base plate is in the closed position, the vessels are tilted at an angle. By tilting the vessels at the angle, the solutions are provided with a greater surface area, which increases the rate of drying.
A unique hinging system is disclosed which hinges each base plate so that is rotates about a pivoting point that is relatively distant from the corresponding manifold. This ensures that the downwardly extending tubes can extend into the vessels when the base plate is moved into the closed position, without the downwardly extending tubes contacting the vessels.
A base can be employed which permits multiple manifold and base plate assemblies to extend therefrom. The base permits the entire dryer manifold to be supported by a small surface area. The present invention is thus highly scalable in that the dryer manifold can include a plurality of manifolds and base plate assemblies. In an exemplary embodiment, the dryer manifold includes two, substantially mirror image, manifold and base plate assemblies, wherein each base plate can hold an array of vessels.
Where multiple manifold and base plate assemblies are employed, a duct system can be utilized to provide gas to the assemblies. One or more inlet heaters can be disposed within the duct system to heat the gas.
The present invention can employ an optional vapor recovery system which recovers exhaust vapors from the one or more vessels that contain solutions to be dried. The optional vapor recovery system can, for example, include a conventional vapor recovery system disposed downstream of the dryer manifold. In addition, or alternatively, the optional vapor recovery system can include a coaxial tube system that prevents exhaust vapors from a vessel from contaminating a solution in another vessel.
In order to control the drying of solutions in vessels, the present invention includes an electrical control system that can adjust the pressure and temperature of the gas and/or the temperature of the solutions to be dried. In an exemplary embodiment, the electrical control system includes one or more open-loop systems, such as manual adjustments, which control the pressure and temperature of the gas and/or the temperature of the solutions to be dried. In another exemplary embodiment, the electrical control system includes one or more closed-loop systems that control temperatures and pressures, based on comparisons of measured values and predetermined values. In another exemplary embodiment, the electrical control system is a combination of open-loop and closed-loop systems.
The present invention can substantially prevent bumping and boiling of the solution in the vessel by controlling the pressure and temperature of the gas and/or the temperature of the solutions, based on the level of solution in a vessel. For example, when a solution level is high, one or more of the pressure and temperatures can be set to low settings. When a sufficient amount of the solution dries, the pressure and temperatures can be set to a higher setting. With an open loop electrical control system, a user can manually adjust one or more controls based upon the level of solution in a vessel. In a closed loop electrical control system, the level of solution can be monitored with one or more level detectors and the electrical control system can control the pressure and temperature of the gas and/or the solution temperature, accordingly.
The drying can be terminated by a timer or by a manual control. Alternatively, the present invention can include one or more moisture sensors that sense the moisture content in the vessels and/or in the exhaust vapor. The electrical control system can terminate the process when the moisture content reaches a predetermined level.
Further features and advantages of the present invention, as well as the structure and operation of various embodiments of the present invention, are described in detail below with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS/FIGURES
The foregoing and other features and advantages of the invention will be apparent from the following, more particular description of an embodiment of the invention, as illustrated in the accompanying drawings.
FIG. 1
illustrates a high-level block diagram of a drying system, in accordance with the present invention.
FIG. 2
illustrates a detailed high-level block diagram of an exemplary embodiment of the drying system illustrated in FIG.
1
.
FIG. 3A
illustrates a top, plan view of a Y-branch duct system that can be employed in the present invention.
FIG. 3B
illustrates a perspective view of the Y-branch duct system illustrated in FIG.
3
A.
FIG. 4
illustrates a control panel that can be used as part of an open-loop electrical control system, in accordance with the present invention.
FIG. 5
illustrates a first perspective view of a dual-chamber dryer manifold and the y-branch duct system, in accordance with the present invention.
FIG. 6
illustrates a second perspective view of the dryer manifold illustrated in FIG.
5
.
FIG. 7
illustrates a third perspective view of the dryer manifold illustrated in
FIGS. 5 and 6
.
FIG. 8
illustrates a vessel tray that can be employed by the present invention.
FIG. 9
illustrates a partially sectional view of the dryer manifold taken along a line
9
—
9
in FIG.
7
.
FIG. 10
illustrates a partially sectional view of the dryer manifold taken along the line
9
—
9
in FIG.
7
.
FIG. 11
illustrates downwardly extending hollow tubes that can be employed by the present invention.
FIG. 12
illustrates a vessel in an upright position holding a solution to be dried.
FIG. 13
illustrates the vessel of
FIG. 12
, tilted at an angle α.
FIG. 14
illustrates a perspective view of a hollow, coaxial vapor recovery tube that can be employed in the present invention.
FIG. 15
illustrates a partially sectioned view of the hollow, coaxial vapor recovery tube illustrated in FIG.
14
.
FIG. 16
illustrates a high-level block diagram of a combination open-loop and closed-loop electrical control system, in accordance with the present invention.
FIG. 17A
is a schematic diagram illustrating a substantially open-loop electrical control system, in accordance with the present invention.
FIG. 17B
is a schematic diagram illustrating an embodiment of a portion of the schematic diagram illustrated in FIG.
17
A.
FIG. 18
is a process flow-chart of a method for drying solutions.
FIG. 19
illustrates a perspective view of a T-branch duct system that can be employed in the present invention.
FIG. 20
is a front plan view of the T-branch duct system illustrated in FIG.
19
.
FIG. 21
is a top plan view of the T-branch duct system illustrated in
FIGS. 19 and 20
.
FIG. 22
illustrates a perspective view of a small footprint drying system that employs the T-branch duct system of
FIGS. 20 and 22
.
FIG. 23
illustrates a front plan view of the system illustrated in FIG.
22
.
FIG. 24
illustrates atop plan view of the system illustrated in
FIGS. 22 and 23
.
FIG. 25
illustrates a vapor recovery plate that can be employed to reduce contamination of solutions in vessels.
FIG. 26
illustrates an array of vessels that can be used to hold solutions to be dried.
DETAILED DESCRIPTION OF THE INVENTION
I. General Overview
The present invention is now described with reference to the figures. While specific configurations and arrangements are discussed, it should be understood that this is done for illustrative purposes only. A person skilled in the relevant art will recognize that other configurations and arrangements can be used without departing from the spirit and scope of the invention.
In the figures, like reference numbers generally indicate identical, functionally similar, and/or structurally similar elements. The figure in which an element first appears is indicated by the leftmost digit(s) in the reference number.
Referring to
FIG. 1
, a drying system
102
includes a dryer manifold
124
that dries solutions contained in one or more arrays of vessels by directing gas
110
, which can be inert gas, air, oxygen, nitrogen, or any other gas or mixture of gasses that are suitable for drying, into the vessels. The solutions can be, for example, solutions that contain macro-molecules including, but not limited to, DNA, proteins, lipids, carbohydrates, RNA, oligonucleotides, polypeptides, cells, antibiotics, chemical compounds, enzymes (DNA or RNA polymerases such as thermostable DNA polymerases including Taq, Tma, or Tne DNA polymerases, restriction endonucleases, ligases, reverse transcriptases, etc.), antibodies or combinations thereof. The solutions can also be, for example, liquid reagents used in diagnostic applications, assays used in clinical environments or assays used in research applications.
In an exemplary embodiment, system
102
includes a filter
112
, that receives and filters gas
110
to generate filtered gas
114
. A fan
116
pressurizes gas
140
to generate filtered, pressurized gas
118
. A heater
120
heats filtered, pressurized gas
118
to generate filtered, pressurized, heated gas
122
. In this embodiment, gas
110
is provided to dryer manifold
124
as filtered, pressurized, heated gas
122
.
One skilled in the relevant art will recognize that one or more of filter
112
, fan
116
and heater
120
can be arranged in a variety of manners. Moreover, one or more of filter
112
, fan
116
and heater
120
can be omitted. Thus, throughout the remainder of this disclosure, it is to be understood that the phrases gas
110
, gas
114
, gas
118
, gas
122
and inlet gas are generally used interchangeably. Unless otherwise noted, each of these terms are used broadly to refer to any type of gas, including, but not limited to, filtered gas, pressurized gas, heated gas, etc., or any combination thereof.
Dryer manifold
124
holds a plurality of vessels (not shown in
FIG. 1
) which contain solutions to be dried and directs gas
110
into the vessels. In an exemplary embodiment, dryer manifold
124
directs gas
110
substantially toward the surface of the solutions to be dried. In an alternative embodiment, dryer manifold
124
directs gas
110
substantially horizontal to the surface of the solutions to be dried. Gas
110
induces evaporation of the solutions, which generates exhaust vapors
126
. The process leaves substantially dry macromolecule substances in the vessels.
Exhaust vapors
126
can be vented into the atmosphere. Alternatively, exhaust vapors
126
can be recovered by an optional vapor recovery system. The optional vapor recovery system can include, for example, a conventional vapor recovery system
128
, downstream of dryer manifold
124
. Additionally, or alternatively, the optional vapor recovery system can include elements within dryer manifold
124
, such as elements that prevent exhaust vapors
126
that exit one vessel from contaminating solutions in other vessels.
In an exemplary embodiment, dryer manifold
124
heats the solutions to be dried in order to further speed the drying process. In an exemplary embodiment, the vessels containing solutions to be dried are tilted on an angle to increase an exposed surface area of the solutions, thereby increasing evaporation rates of the solutions.
An optional electrical control system
130
provides power and control signals to one or more of fan
116
, heater
120
, dryer manifold
124
and vapor recovery system
128
. In an exemplary embodiment, electrical control system
130
is an open-loop system that includes manually operated controls to control, for example, a speed of fan
116
, a temperature of heater
120
and/or a temperature of dryer manifold
124
.
In an alternative exemplary embodiment, electrical control system
130
is a closed-loop system that receives electrical signals representative of, for example, a pressure of gas
122
, a temperature of gas
122
and/or a temperature of dryer manifold
124
. The closed loop electrical control system
130
compares one or more of the received signals to signals indicative of, for example, desired pressures and/or temperatures. The closed loop electrical control system
130
can adjust a speed of fan
116
, a temperature of heater
120
and/or a temperature of dryer manifold
124
, accordingly. In another alternative exemplary embodiment, electrical control system
130
is a combination of open loop and closed loop system.
II. Example Embodiment
Referring to
FIG. 2
, a high-level block diagram of an embodiment of drying system
102
is illustrated. In this embodiment, dryer manifold
124
is a dual-manifold assembly that includes a front chamber
212
and a rear chamber
214
. Chambers
212
and
214
each hold a plurality of vessels (not shown in
FIG. 2
) that contain solutions to be dried. The vessels can be arranged in a plurality of arrays of vessels. Chambers
212
and
214
receive gas
122
through a duct system
210
.
Filter
112
is illustrated as a high extraction particulate air (HEPA) filter. HEPA filters are well known in the relevant art. A variety of types of HEPA filters can be employed, as would be apparent to one skilled in the relevant art.
Fan
116
is illustrated as a fan blower motor that draws gas
110
through HEPA filter
112
and outputs pressurized, filtered gas
118
. Fan blower motor
116
can be a variety of commercially available, off-the-shelf fan blower motors. Alternatively, fan blower motor
116
can be custom designed to desired specifications.
One skilled in the relevant art will recognize that a variety of combinations of off-the-shelf or custom HEPA filters
112
and fan blower motors
116
can be employed in the present invention. Conventional, off-the-shelf systems that combine a HEPA filter
112
with a fan blower motor
116
can also be used.
Pressurized, filtered gas
118
is provided to duct system
210
. Referring to
FIGS. 19-21
, an exemplary embodiment of duct system
210
is illustrated as a T-branch duct system
1910
. T-branch duct system
1910
includes a common branch (T-branch)
1912
that divides filtered, pressurized gas
118
between a front branch
1914
and a rear branch
1916
. Branches
1914
and
1916
can be constructed from, for example, three inch diameter flexible silicone duct tubes. Other diameters can be used, as would be apparent to one skilled in the relevant art. Actual dimensions can vary with implementations.
A first end
1913
of front branch
1914
can be adjustably coupled to T-branch
1912
by a compression fitting
1920
. A second end
1915
of front branch
1914
can be adjustably coupled to an end plate
1918
of dryer manifold
124
by a compression fitting
1922
. Rear branch
1916
can be coupled between T-branch
1912
and end plate
1918
in a similar fashion.
Referring to
FIGS. 22-24
, in an exemplary embodiment, T-branch duct system
1910
can be configured so that HEPA filter
112
and/or fan
116
rest on a top plate
2214
of dryer manifold
124
(
FIGS. 5-7
,
9
and
10
). In this embodiment, front branch
1914
includes a pivoting section
2210
that permits front branch
1914
to pivot with respect to end plate
1918
. Likewise, adjustable compression fitting
1920
permits T-branch
1912
to pivot with respect to front branch
1914
. Rear branch
1916
includes a similar pivoting section
2212
. This configuration reduces the overall footprint of system
102
.
Referring to
FIGS. 3A and 3B
, in an alternative exemplary embodiment, duct system
210
is illustrated as a Y-branch duct system
310
. Y-branch duct system
310
includes a common branch (Y-branch)
312
that receives and divides gas
118
between a front branch
314
and a rear branch
316
.
Referring back to
FIG. 2
, duct system
210
can include a first heater
120
in a front branch
230
and a second heater
120
in a rear branch
232
. Front branch
230
can be front branch
1914
of T-branch duct system
1910
or front branch
312
of Y-branch duct system
310
. Rear branch
232
can be rear branch
1916
of T-branch duct system
1910
or rear branch
314
of Y-branch duct system
310
. A single heater
120
(not shown) could be provided in front branch
230
and rear branch
232
.
Heater(s)
120
can be a variety of conventional, off-the-shelf heaters, such as geometrically-reformable heaters available from Watlow Electrical Manufacturing Co. of St. Louis, Mo. Geometrically-reformable heaters can be formed into a variety of shapes, such as a compact coiled nozzle, a straight cable, a flat spiral, a star-wound, etc. Heater(s)
120
can be secured within duct system
210
with a variety of conventionally known techniques, such as bolts, screws, epoxy, etc.
Duct system
210
provides gas
122
to chambers
212
and
214
. Duct system
210
provides scalability in that a plurality of drying chambers can be employed to dry solutions in vessels. One skilled in the relevant art will recognize that a variety of types of duct systems
210
can be employed.
In an exemplary embodiment, chambers
212
and
214
include heaters
216
and
218
, respectively, for heating the vessels. Heaters
216
and
218
can be a variety of conventional, off-the-shelf heaters. For example, heaters
216
and
218
can include tapes, mats, fine-strand resistance wires insulated and enclosed in high-strength, high-temperature-resistant silicone rubber, etc. Silicone rubber heaters are available as tapes and mats from, for example, Cole-Parmer Instrument Company, of Vernon Hills, Ill. A silicone heating mat, available from Cole-Parmer as part no. E-03125-50, for example, can be used.
In operation, gas
110
is provided to front chamber
212
and to rear chamber
214
by front and rear branches
230
and
232
, respectively, of duct system
210
. Gas
110
is passed over the solutions to be dried and into an exhaust chamber
220
as exhaust vapors
126
. Exhaust vapors
126
are removed from exhaust chamber
220
, via an exhaust duct
222
. Exhaust duct
222
can include an optional exhaust fan (not shown). Exhaust vapors
126
can be sent to an optional vapor recovery system
128
(not shown in FIG.
2
).
Electrical control system
130
controls one or more of fan
116
and heaters
120
,
216
and
218
. Electrical control system
130
can include, for example, one or more dual-zone heater controllers
224
to control heaters
120
,
216
and
218
. Electrical control system
130
can also include an AC motor controller
228
to control fan blower motor
116
.
A pressure switch (not shown) can be provided downstream of fan
116
to measure the pressure of gas
118
or
122
. In an embodiment, electrical control system
130
does not energize heaters
120
,
216
and
218
until a predetermined pressure is sensed by the pressure switch. This prevents heat-induced damage to system
102
in the event that fan blower motor
116
fails.
Electrical control system
130
can include a digital timer
226
to delay sampling of the pressure switch for a predetermined period of time. This provides fan blower motor
116
with the predetermined period of time to get up to speed before electrical control system
130
can declare a low pressure fault.
A. Dryer Manifold
124
Referring to
FIGS. 5
,
6
and
7
, dryer manifold
124
is illustrated as a dual-chamber dryer manifold, including front chamber
212
and rear chamber
214
. Chamber
214
is a substantially mirror image of chamber
212
.
FIGS. 5 and 6
illustrate partial cutaway views of dual-chamber dryer manifold
124
. Front chamber
212
includes a manifold
510
and a base plate
512
.
Referring to
FIG. 6
, base plate
512
can hold one or more vessels
614
. In an exemplary embodiment, vessels
614
are held by one or more vessel trays
612
. Vessel trays
612
can be removably placed on base plate
512
. Referring to
FIG. 8
, vessel trays
612
can include an array of vessel cavities
810
that receive vessels
614
. Vessels
614
can be press-fitted vessels that are held in place by friction. Vessels
614
can be made from, for example, thermoplastics and/or metal and can be, for example thin-walled stainless steel vessels.
Referring to
FIG. 26
, in an embodiment, an array of vessels
614
can be provided as one or more deep-well plates of vessels
2610
, such as deep-well plates available from Beckman Instruments, Inc. of King of Prussia, Pa. For example, part number 227006 from Beckman Instruments includes an array of twenty-four, one milliliter wells. A lid
2612
can be used to seal vessels
2612
when solutions in deep well plate
2610
are not being dried.
Referring back to
FIG. 6
, base plate
512
can include a recessed portion
616
for receiving one or more of vessels
614
, vessel trays
612
, deep well plates
2610
, etc. Recessed portion
616
can be designed to receive any number vessels
614
, vessel trays
612
, deep well plates
2610
, etc. Vessel trays
612
and deep well plates
2610
can hold any number of vessels
614
. Base plate
512
can include a recessed perimeter
622
for receiving a seal, such as a silicone o-ring seal
624
.
In an exemplary embodiment, dryer manifold
124
heats solutions in vessels
614
. For example, base plate
512
can include a heater
216
to heat solutions in vessels
614
. Heater
216
can be implemented as, for example, a thin, silicone-sealed heating pad placed in recessed portion
616
so that vessel trays
612
rest thereon. The heating pad can be connected to an electrical source via leads
618
. Alternatively, any other suitable heat source can be used to heat solutions in vessels
614
. For example, solutions in vessels
614
can be heated with a radiant heater (not shown), a heating coil embedded within base plate
512
(not shown), etc.
Base plate
512
, vessel trays
612
and/or deep-well plates of vessels
2610
can be fabricated from metals such as aluminum alloys and coated aluminum alloys, from thermoplastics such as polypropylene and that sold by DuPont Co. of DE under the trademark Delrin, etc., or combinations thereof. Where dryer manifold
124
heats solutions in vessels
614
, one or more portions dryer manifold
124
are preferably manufactured from materials that do not readily transfer heat (eg., thermoplastics, etc.). This ensures better control over heating of solutions in vessels
614
.
Referring to
FIG. 7
, dryer manifold
124
includes a base
710
. Base
710
is common to front and rear chambers
212
and
214
. In the illustrated embodiment, base plate
512
is hingedly coupled to base
710
by hinges
712
. Hinges
712
provide dryer manifold
124
(or base plate
512
) with an open position and a closed position. In both FIG.
5
and
FIG. 6
, base plate
512
is illustrated in the open position. In
FIG. 7
, base plate
512
is illustrated in the closed position. When in the closed position, base plate
512
is sealing engagement with manifold
510
.
In an exemplary embodiment, manifold
510
includes a front wall
714
, a rear wall
716
, a first end wall
718
and a second end wall
720
. In the illustrated embodiment, front chamber
212
has rectangular shape. Alternatively, front chamber
212
can be designed in a variety of other shapes.
Referring back to
FIG. 6
, manifold
510
includes a nozzle plate
628
which has an array of passages
630
. Manifold
510
also includes a baffle plate
632
that guides gas
110
from an inlet
634
through passages
630
. Baffle plate
632
and nozzle plate
628
define a plenum
640
therebetween. Referring to
FIG. 10
, when base plate
512
is in the closed position, nozzle plate
628
and base plate
512
form a cavity
1010
therebetween.
Referring back to
FIG. 6
, nozzle plate
628
includes hollow tubes
636
extending downwardly from passages
630
. Referring to
FIG. 10
, dryer manifold
124
is designed so that, when base plate
512
is in the closed position, hollow tubes
636
extend into vessels
614
, without touching vessels
614
or the solutions therein.
In operation, gas
110
passes through inlet
634
and into plenum
640
, where baffle plate
632
forces gas
110
downwardly through passages
630
and through hollow tubes
636
. Preferably, hollow tubes
636
do not extend so far into vessels
614
that they contact the solution to be dried. Instead, gas
110
is emitted under pressure from hollow tubes
636
and passes over the surface of the solutions to be dried. As gas
110
passes over the surface of the solutions to be dried, the solutions evaporate, generating exhaust vapors
126
. Exhaust vapors
126
pass through an exhaust passage
1012
, into exhaust chamber
220
and out an exhaust
642
(FIG.
6
).
In an exemplary embodiment, baffle plate
632
is at an angle of 14.25 degrees relative to nozzle plate
628
. This ensures adequate gas flow through all of passages
630
. The angle can, however, be set or adjusted to any suitable angle.
Referring to
FIG. 11
, downwardly extending hollow tubes
636
can be fashioned in a variety of designs. In an exemplary embodiment, a hollow tube
636
a
includes a substantially downwardly directed opening
1110
that directs gas
110
substantially at a surface
1112
of solution
1114
. In another exemplary embodiment, a hollow tube
636
b
, includes one or more horizontally directed openings
1116
that direct gas
110
substantially horizontal to surface
1112
. Hollow tube
636
b
can be employed, for example, to reduce foaming and bumping of solution
1114
. Openings
1110
and
1116
can be combined on a single hollow tube (not shown). One skilled in the relevant art will recognize that a variety of other options can be employed as well.
The present invention can reduce drying times by increasing a surface area of a solution to be dried. Referring to
FIG. 12
, vessel
614
is illustrated in an upright position. This is the position of vessel
614
when base plate
512
is in the open position, as illustrated in
FIGS. 5 and 6
. Referring to
FIG. 13
, vessel
614
is illustrated tilted at an angle α. This is the position of vessel
614
when base plate
512
is in the closed position, as illustrated in
FIGS. 7
,
9
and
10
.
Tilting vessels
614
at an angle increases the surface area of the solution to be dried and thus speeds the drying process. When vessel
614
is upright, as illustrated in
FIG. 12
, solution
1114
has a surface area
1112
a
. When vessel
614
is tilted as illustrated in
FIG. 13
, surface area
1112
a
increases to
1112
b
. As is well known to those skilled in the art, increasing the surface area of the solution to be dried in vessel
614
increases the rate of evaporation of the solution
1114
. In an exemplary embodiment, base plate
512
, and hence vessel tray
612
and vessel
614
, are tilted at an angle α of twenty-five degrees. Alternatively, α can be any angle so long as solution
1114
does not spill out of vessel
614
.
Through a combination of increasing the surface area
1112
of solutions to be dried, heating solutions to be dried, and directing heated gas over the solutions to be dried, drying times are substantially reduced as compared to conventional systems. For example, the present invention can drys plates of forty-eight vessels, each vessel containing 0.5 ml of aqueous solutions in about forty-five to about sixty minutes. A conventional drying system, such as the type constructed by Savant Instruments, which uses a vacuum pump and centrifuge connected to a refrigerated vapor trap, takes three to four hours to dry the same volumes of aqueous solutions.
B. Vapor Recovery
In an exemplary embodiment of the present invention, a vapor recovery system is used to capture exhaust
126
vapors that are evaporated from solution
1114
and/or that are introduced by gas
110
. Referring to
FIGS. 1 and 2
, a conventional vapor recovery system
128
can be provided downstream of exhaust chamber
220
. In addition, or alternatively, coaxial vapor recovery systems can be employed to prevent exhaust vapors
126
from one vessel
614
from interacting with solutions in another vessel
614
. Coaxial vapor recovery systems also serve to prevent solution loss and contamination from foaming and bumping.
Referring to
FIG. 25
, in an exemplary embodiment, a vapor recovery plate
2510
is disposed with front chamber
212
, below and substantially parallel to nozzle plate
628
, forming a head space
2512
therebetween. Vapor recovery plate
2510
, and passages
2514
therethrough, are designed to reduce or eliminate exhaust vapors
126
from a vessel
614
from entering, and possibly contaminating, another vessel
614
. Vapor recovery plate
2510
includes an array of passages
2514
, each having a first end
2516
that opens to head space
2512
and a second end
2518
that opens to cavity
1010
. The shape and size of second end
2518
substantially matches the shape and size of an opening
812
(
FIG. 8
) of vessels
614
. When base plate
512
is in the closed position, vapor recovery plate
2510
forms a tight, compression-like fit with vessels
614
. Hollow tubes
636
extend through passages
2514
so that gas
122
passes from plenum
640
, through tubes
636
and into vessels
614
. Exhaust vapors
126
rise from vessels
614
through passages
2514
(outside of hollow tubes
636
) and into head space
2512
. From head space
2512
, exhaust vapors
126
exit through exhaust passages
1012
.
Referring to
FIG. 14
, another exemplary embodiment of a coaxial vapor recovery system includes a coaxial hollow tube
1410
that extends from a nozzle passage
630
(FIG.
6
). Coaxial hollow tube
1410
includes a pipette
1414
that can be similar to hollow tubes
636
a
and/or
636
b
, illustrated in FIG.
11
. Coaxial hollow tube
1410
includes an outer tube, or collar,
1416
having a seat
1418
. When base plate
512
is in the closed position, seat
1418
is in sealing engagement with a rim
1420
of vessel
614
. In operation, gas
122
enters a top opening
1426
of pipette
1414
and exits pipette
1414
from a lower opening
1422
to interact with surface
1112
of solution
1114
. Portions of solution
1114
evaporate as exhaust vapors
126
and exit out of an opening
1424
of collar
1416
. Collar
1416
substantially prevents exhaust vapors
126
from other vessels
614
from entering the vessel
614
illustrated in FIG.
14
.
Referring to
FIG. 15
, a partial cutaway view of nozzle plate
628
and vessel tray
612
is illustrated. Exhaust vapors
126
that exits from exhaust opening
1424
a
can be captured by a hose
1510
coupled thereto. Alternatively, outer tube
1416
can be embedded within nozzle plate
628
, where opening
1424
b
coincides with a passage
1512
, within nozzle plate
628
, that leads to exhaust passage
1012
.
C. Electrical Control System
130
Electrical control system
130
controls the drying of solutions in vessels
614
by controlling one or more of the pressure and temperature of gas
122
and the temperature of solutions
1114
. In an exemplary embodiment, electrical control system
130
is a closed-loop system that controls one or more of the pressure and temperature of gas
122
and the temperature of solutions
1114
, based on comparisons between measured values and predetermined values. In another embodiment, electrical control system
130
is an open-loop system that includes manual adjustments for controlling one or more of the pressure and temperature of gas
122
and the temperature of solutions
1114
. In another embodiment, electrical control system
130
is a combination open-loop and closed-loop system.
Referring to
FIG. 16
, a high-level block diagram illustrates electrical control system
130
as a combination open-loop and close-loop system
1602
. Electrical control system
1602
uses an open-loop portion
1604
to control fan blower motor
116
and a close-loop portion
1606
to control the temperatures of gas
122
and solutions
1114
.
In operation, an alternating current (AC) mains voltage
1608
supplies electrical power to digital timer
226
. Digital timer
226
supplies electrical power to solid state AC power controller
1612
, which provides power to fan blower motor
116
. After a delay, digital timer
226
also supplies electrical power to a pressure switch
1614
. The delay permits fan
116
to get up to speed before heat is applied to the system. Pressure switch
1614
is positioned downstream of fan blower motor
116
to measure the pressure of gas
122
. When the pressure of gas
122
reaches a predetermined level, pressure switch
1614
closes a circuit that supplies electrical power to programmable interface dual-zone (PID) controller
1616
.
PID controller
1616
controls the temperatures of solutions
1114
and gas
122
. PID controller
1616
controls the temperature of solutions
1114
by comparing a signal indicative of a measured temperature with a signal indicative of a desired temperature of solutions
1114
. For example, PID controller
1616
can receive a signal
1618
from a thermocouple heat sensor
1620
that is positioned within cavity
1010
. Preferably, thermocouple heat sensor
1620
is positioned within cavity
1010
so that it is in physical contact with at least one vessel
614
or vessel tray
612
. PID controller
1616
compares signal
1618
with a signal (not shown) that represents the desired temperature of solutions
1114
. PID controller
1616
adjusts the temperature of heating elements
216
,
218
, according to the results of the comparison.
PID controller
1616
can be, for example, a PID controller available from Watlow Systems Integrators Co. of Decorah, Iowa, as part number DUAL-1JRX-200C. Suitable thermocouple sensors
1620
(i.e., temperature probes) include, for example, surface probes available from Cole-Parmer Instrument Company as part number E-08517-63. One skilled in the relevant art will recognize that a variety of PID controllers and temperature probes can be employed.
PID controller
1616
can control heaters
120
in a similar fashion. For example, PID controller
1616
can receive one or more signals
1626
indicative of a temperature of gas
122
. Signals
1626
can be output from one or more thermocouple sensors
1622
that are disposed downstream of heaters
120
. Signals
1626
can be compared to one or more signals (not shown) that are indicative of a desired temperature of gas
122
. Based on the comparison, PID controller
1616
can control the temperature of heaters
120
. Thermocouple sensors
1622
can be, for example, heater probes available from Cole-Parmer as part number E-08519-73. One skilled in the relevant art will recognize that a variety of temperature probes can be employed.
Alternatively, electrical control system
130
can employ open-loop heater controllers in place of closed-loop heater controllers
1616
. For example, AC-power heater controllers available from Cole-Parmer as part number E-03052-65, can be employed. One skilled in the relevant art will recognize that any of a variety of open-loop heater controllers can be employed.
Electrical control system
130
can include a variety of optional features. For example, referring back to
FIG. 2
, in a closed-loop embodiment of electrical control system
130
, one or more level detectors
236
can be used to measure the level of solution
1114
in one or more vessels
614
. Based on a measured level, electrical control system
130
can control one or more of the pressure and temperature of gas
122
and the temperature of solutions
1114
.
For example, when a solution level is at a high level, electrical control system
130
can set the pressure and/or temperature of gas
122
and/or the temperature of solutions
1114
to a low setting. This serves to reduce or prevent loss of solution due to foaming and bumping. When a sufficient amount of the solution dries, as detected by the level detector, the electrical control system can reset the pressure and temperature of gas
122
and the temperature of solutions
1114
to a higher setting.
Still referring to
FIG. 2
, another optional feature includes one or more moisture sensors
234
that sense the moisture content of solutions
1114
. Moisture sensors
234
can be positioned within or downstream of drying chamber
124
. Electrical control system
130
can terminate the drying process when the moisture content is reduced to a predetermined level. Alternately, the drying process can be terminated by a timer or can be terminated manually.
Referring to
FIGS. 17A and 17B
, electrical control system
130
is illustrated as a substantially open-loop control system
1710
. The following disclosure includes references to
FIG. 4
, where a control panel
410
includes a variety of displays and manual adjustments for controlling gas temperature and pressure and solution temperature.
In
FIG. 17A
, AC power is supplied to a terminal block
1712
. AC power can be applied to terminal block
1712
through, for example, a protective fuse
1714
and a manual on/off switch
1716
.
A voltage controller
1726
receives AC power from terminal block
1712
and controls fan
116
. Voltage controller
1726
can include a manual on/off switch
1728
and a manually adjustable control
1732
to control the speed of fan
116
. A protective fuse
1730
disconnects power from voltage controller
1726
and fan
116
in the event of an over current draw. Manually adjustable control
1732
, which is illustrated as control
412
in
FIG. 4
, can be, for example, an adjustable resistor.
A second voltage controller
1734
receives AC power from terminal block
1712
and controls the temperature of heating elements
216
and
218
. Second voltage controller
1734
includes a manually adjustable control
1736
that controls heating elements
216
and
218
. Manually adjustable control
1736
, which is illustrated as control
414
in
FIG. 4
, can be, for example, an adjustable resistor.
Referring to back to
FIGS. 17A and 17B
, a rectifier circuit
1718
supplies DC power to a pressure sensor
1720
and to one or more temperature sensors
1722
. Pressure sensor
1720
is disposed downstream of fan
116
to measure the pressure of gas
118
. Temperature sensors
1722
can include a first temperature sensor disposed downstream of heater
120
to measure the temperature of gas
122
and/or a second temperature sensor that measures the temperature of solutions
1114
. One skilled in the relevant art will recognize that a variety of temperature probes can be employed, such as temperature probes available from Cole-Parmer.
In
FIG. 4
, a display
418
, which can be a liquid crystal display (LCD), provides a visual indication of the temperature of solutions
1114
. A display
420
provides a visual indication of the gas temperature. Panel meters
418
and
420
can be, for example, panel meters available from Cole-Parmer.
Pressure sensor
1720
and temperature sensors
1722
control a relay circuit
1724
. When pressure sensor
1720
senses sufficient gas flow from fan
116
, and when inlet gas temperature sensors
1720
do not sense an over-limit temperature, current flows through coil
1746
of relay
1724
. Coil
1746
closes normally open contact
1748
, which provides AC power to third voltage controller
1742
.
Third voltage controller
1742
includes a manually adjustable control
1744
that controls the temperature of heater(s)
120
. Manually adjustable control
1744
, which is illustrated as control
416
in
FIG. 4
, can be, for example, an adjustable resistor.
In another embodiment, relay
1724
can also control AC power to second voltage controller
1734
, so that heaters
216
and
218
cannot be energized unless sufficient gas flow is detected by pressure sensor
1720
.
In
FIG. 4
, controls
412
,
414
and
416
permit a user to control the rate of drying of solutions
1114
and to reduce or prevent bumping and boiling of the solutions
1114
by adjusting gas pressure, gas temperature and/or solution temperature. For example, when there is a relatively large amount of a solution
1114
in a vessel
614
, the user can set gas pressure, gas temperature and/or solution temperature to low levels. When a sufficient amount of solution
1114
has evaporated, the user can set gas pressure, gas temperature and/or solution temperature to high levels.
One skilled in the relevant art will recognize that an open-loop electrical control system
130
and a closed-loop electrical control system
130
can be implemented in a variety of fashions using a variety of commercially-available and/or design specific hardware, software, firmware or any combination thereof.
II. Method for Drying Solutions
Referring to the process flowchart of
FIG. 18
, a method for drying solutions is provided. The process is described herein as performed by system
102
. It will be apparent to one skilled in the relevant art, however, that the process illustrated in
FIG. 18
can be performed by a variety of systems. Thus, operation of the present invention is not intended to be limited to the apparatus described with reference to system
102
.
The process begins at a step
1802
, where gas
110
is filtered. Gas
110
can be inert gas, air, oxygen, nitrogen, or any other gas or mixture of gasses that are suitable for drying solutions
1114
. Step
1802
can be performed by HEPA filter
112
as illustrated in FIG.
2
. Electrical control system
130
can include a filter monitor (not shown) that provides an indication, such as a visual indication, when one or more filter elements (not shown) within filter
112
need to be replaced.
In a step
1804
, gas
110
is pressurized by fan
116
. Electrical control system
130
can include a pressure switch downstream of fan
116
that can sense under-pressure and over-pressure conditions, so that electrical control system
130
can adjust the speed of fan
116
. Steps
1802
and
1804
can be performed by a single, off-the-shelf, combination HEPA filter and fan blower motor.
In a step
1806
, gas
110
is heated by one or more heaters
120
. Heaters
120
can be located within duct system
210
. Electrical control system
130
can include heat sensors downstream of heaters
120
that monitor the temperature of gas
110
. A heater controller, such as a PID controller
1616
, can automatically adjusts a voltage or current to heaters
120
in order to maintain gas
110
at a desired temperature. Alternatively, heaters
120
can be controlled with a manually adjustable control
1744
.
In a step
1808
, an array of solution-containing vessels
614
are heated. In an exemplary embodiment, one or more vessel trays
612
are placed on a heated surface of base plate
512
.
One skilled in the relevant art will recognized that steps
1802
-
1808
can be performed in any suitable order. In addition, one or more of steps
1802
-
1808
can be omitted.
In a step
1810
, gas
110
, which can be heated, pressurized, filtered gas
122
, is directed into vessels
614
. For example, in
FIG. 6
, gas
110
is provided to plenum
640
, via inlet
634
. Plenum
640
directs gas
110
downwardly through passages
630
, through hollow tubes
636
and into solution-filled vessels
614
.
In an exemplary embodiment, gas
110
exits hollow tubes
636
a
and imparts substantially directly upon a surface
1112
of solution
1114
. In another embodiment, gas
122
exits hollow tubes
636
b
substantially horizontal to surface
1112
.
In order to increase the rate of evaporation of solution
1114
, solution-filled vessels
614
can be tilted at an angle, as illustrated in
FIG. 13
, to increase the exposed surface area
1112
b
. In an exemplary embodiment, vessels
614
are tilted at an angle of about twenty-five degrees.
In a step
1812
, exhaust vapors
126
are removed from vessels
614
. In an exemplary embodiment, exhaust vapors
122
are forced from vessels
614
, through exhaust duct
222
, under pressure from fan
116
. Additionally, or alternatively, an exhaust fan (not shown) can be disposed downstream of dryer manifold
124
to draw exhaust vapors
126
away from vessels
614
.
At this point, processing can proceed through a variety of options. In an exemplary embodiment, steps
1802
-
1812
are performed for a set period of time, such as 45 minutes, for example. At the end of the set period of time, processing stops at step a
1814
.
Alternatively, in a step
1816
, electrical control system
130
determines whether solutions
1114
are dry. For example, one or more moisture meters
234
can be installed within each of front chamber
212
and rear chamber
214
. Alternatively, a single moisture meter
234
can be disposed downstream of dryer manifold
124
. While the moisture level remains above a predetermined level, steps
1802
-
1812
are performed as a continuous loop. When the moisture level drops below the predetermined level, processing proceeds to and stops at step
1814
.
Another option is vapor recovery. In a step
1818
, exhaust vapors
126
are recovered. In an embodiment, exhaust vapors
122
can be received by a conventional vapor recovery system
128
. In another embodiment, a coaxial vapor recovery system can be employed to substantially prevent exhaust vapors
126
exiting a vessel
614
from contaminating a solution
1114
in another vessel
614
,. For example, vapor recovery plate
2510
can be employed. As another example, coaxial tubes
1410
can be employed.
In a step
1820
, recovered exhaust vapors
126
are processed. Processing can include processing in accordance with state or federal environmental protection regulations, in accordance with industry standards, in accordance with any other standards, or any combination thereof.
Processing proceeds to, and stops at, step
1814
.
III. Conclusions
While the invention has been particularly shown and described with reference to preferred embodiments thereof, it will be understood by those skilled in the relevant arts that various changes in form and details can be made therein without departing from the spirit and scope of the invention.
Claims
- 1. A method for drying a solution containing macromolecules, comprising the steps of:(1) receiving a vessel containing the solution; (2) directing a gas into the vessel; (3) sensing a moisture content of the solution; and (4) terminating step (2) when the moisture content of the solution reaches a predetermined level.
- 2. The method according to claim 1, further comprising the step of:(5) filtering the gas.
- 3. The method according to claim 1, further comprising the step of:(5) heating the gas.
- 4. The method according to claim 3, further comprising the steps of:(6) monitoring a temperature of the gas; and (7) adjusting the temperature of the gas to correspond to a desired temperature.
- 5. The method according to claim 1, further comprising the step of:(5) pressurizing the gas.
- 6. The method according to claim 5, further comprising the steps of:(6) monitoring a pressure of the gas; and (7) adjusting the pressure of the gas to correspond to a desired pressure.
- 7. The method according to claim 1, further comprising the step of:(5) heating the solution in the vessel.
- 8. The method according to claim 7, further comprising the step of:(6) monitoring a temperature of the solution; and (7) adjusting the temperature of the solution to correspond to a desired temperature.
- 9. The method according to claim 1, further comprising the step of:(5) performing steps (1)-(4) on a plurality of vessels.
- 10. The method according to claim 1, further comprising the step of:(5) tilting the vessel.
- 11. The method according to claim 1, wherein step (2) comprises the step of:(a) directing the gas substantially at the solution.
- 12. The method according to claim 1, wherein step (2) comprises the step of:(a) directing the gas substantially horizontal to the solution.
- 13. The method according to claim 1, further comprising the steps of:(5) heating the solution to a first temperature when a level of the solution is at a first level; and (6) heating the solution to a second temperature when the level of the solution in the vessel is at a second level.
- 14. A method according for drying a solution containing macromolecules, comprising the steps of:(1) receiving a vessel containing the solution; (2) directing a gas into the vessel; (3) pressurizing the gas to a first pressure when a level of the solution is at a first level; and (4) pressurizing the gas to a second pressure when the level of the solution in the vessel is at a second level.
- 15. The method according to claim 14, further comprising the step of:(5) filtering the gas.
- 16. The method according to claim 14, further comprising the step of:(5) heating the gas.
- 17. The method according to claim 16, further comprising the steps of:(6) monitoring a temperature of the gas; and (7) adjusting the temperature of the gas to correspond to a desired temperature.
- 18. The method according to claim 14, further comprising the steps of:(5) monitoring a pressure of the gas; and (6) adjusting the pressure of the gas to correspond to a desired pressure.
- 19. The method according to claim 14, further comprising the step of:(5) heating the solution in the vessel.
- 20. The method according to claim 19, further comprising the steps of:(6) monitoring a temperature of the solution; and (7) adjusting the temperature of the solution to correspond to a desired temperature.
- 21. The method according to claim 14, further comprising the step of:(5) performing steps (1)-(4) on a plurality of vessels.
- 22. The method according to claim 14, further comprising the step of:(5) tilting the vessel.
- 23. The method according to claim 14, wherein step (2) comprises the step of:(a) directing the gas substantially at the solution.
- 24. The method according to claim 14, wherein step (2) comprises the step of:(a) directing the gas substantially horizontal to the solution.
- 25. The method according to claim 14, further comprising the steps of:(5) heating the solution to a first temperature when a level of the solution is at a first level; and (6) heating the solution to a second temperature when the level of the solution in the vessel is at a second level.
- 26. A method for drying a solution containing macromolecules, comprising the steps of:(1) receiving a vessel containing the solution; (2) directing a gas into the vessel; (3) heating the gas to a first temperature when a level of the solution is at a first level; and (4) heating the gas to a second temperature when the level of the solution in the vessel is at a second level.
- 27. The method according to claim 26, further comprising the step of:(5) filtering the gas.
- 28. The method according to claim 26, further comprising the steps of:(5) monitoring a temperature of the gas; and (6) adjusting the temperature of the gas to correspond to a desired temperature.
- 29. The method according to claim 26, further comprising the step of:(5) pressurizing the gas.
- 30. The method according to claim 29, further comprising the steps of:(6) monitoring the pressure of the gas; and (7) adjusting the pressure of the gas to correspond to a desired pressure.
- 31. The method according to claim 26, further comprising the step of:(5) heating the solution in the vessel.
- 32. The method according to claim 31, further comprising the steps of:(6) monitoring a temperature of the solution; and (7) adjusting the temperature of the solution to correspond to a desired temperature.
- 33. The method according to claim 26, further comprising the step of:(5) performing steps (1)-(4) on a plurality of vessels.
- 34. The method according to claim 26, further comprising the step of:(5) tilting the vessel.
- 35. The method according to claim 26, wherein step (2) comprises the step of:(a) directing the gas substantially at the solution.
- 36. The method according to claim 26, wherein step (2) comprises the step of:(a) directing the gas substantially horizontal to the solution.
- 37. The method according to claim 26, further comprising the steps of:(5) heating the solution to a first temperature when a level of the solution is at a first level; and (6) heating the solution to a second temperature when the level of the solution in the vessel is at a second level.
US Referenced Citations (22)
Foreign Referenced Citations (2)
Number |
Date |
Country |
4316163 |
May 1993 |
DE |
202082 |
Feb 1923 |
GB |