Note: Descriptions are shown in the official language in which they were submitted.
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APPARATUS AND METHOD FOR
DISPENSING HIGH PURITY MATERIALS
Field of the Invention
[0001] This invention relates to system or apparatus and a method for
dispensing high purity material from a container without compromising the
purity of
the material. More particularly, the invention relates to a system or
apparatus and a
method for dispensing high purity chemicals, and particularly ultra dry
solvents
intended for use in laboratory scale synthesis studies, from a container, and
particularly from a positive dispense container or can while maintaining the
integrity
of the material.
Background to the Invention
[0002] Numerous dispensing systems are known for dispensing materials
from pressurized containers. The material to be dispensed in the pressurized
container generally provided with a dispensing valve. Upon activation of the
valve a
pressure differential between the internal pressure in the container and the
ambient
pressure permits the dispensing of the material from the container. While such
a
simple system is acceptable for many applications, where the continuing purity
and
integrity of the material to be dispensed is a prime concern, such systems do
not
permit the purity and integrity of the material to be maintained upon
dispensing of
the material. One such material is ultra dry solvent utilized in laboratory
scale
synthesis studies. Such ultra dry solvents are degraded by contact with
moisture
and oxygen.
[0003] For large scale storage. and dispensing of such ultra dry solvents
there
is presently available a CYCLE-TAINER container for a solvent delivery system.
Such system comprises a closed stainless steel container, available in 4, 8,
52, 215
and 1250 liter sizes, containing the material to be dispensed, and is provided
with
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appropriate valving. In use, an inlet valve of the container is hooked up to a
source
of pressurized inert gas, such as argon or nitrogen, and the outlet valve from
the
container is connected to a hose leading directly to the reactor or vessel
where the
stored material is to be employed or used. Upon introduction of the
pressurized gas
into the container the material may be dispensed. Cutting off the source of
inert gas
and closing of the valve stops the dispensing of the material from the
container and
preserves the integrity of the stored material. Such a system is not suitable,
practical or acceptable, however, for conditions where one desires to dispense
only
small quantities of the material from a positive pressurized container, such
as where
one desires to dispense from a pressurized container only about 10 to about 20
mL
of an ultra dry solvent material for lab scale synthesis studies. One way in
which the
art has attempted to solve this problem is to employ a syringe and a septum
sealed
bottle or container that contains, under a blanket of inert gas, the desired
material to
be dispensed. With this type of apparatus it is necessary for the user to
puncture
the septum of the bottle with the needle of a syringe to extract the material
from the
septum container. However, this insertion of the needle into the septum
container
itself can be a cause of contamination of the material and destroy the
integrity of the
material. Additionally, the puncturing of the septum leaves a hole in the
septum
permitting escape of the blanket of inert gas and introduction of atmospheric
gas,
particularly oxygen, and moisture into the material stored in the septum
container.
Thus, there is a definite need for an acceptable dispensing system or
apparatus for
dispensing a material, especially relatively small amount of material, from a
pressurized material that permits the dispensing to occur while maintaining
the purity
and integrity of the material being dispensed.
Summary of the Invention
[0004] This invention relates to a system or apparatus and a method for
dispensing a material from a pressurized container while maintaining product
integrity. The system or apparatus comprises a pressurized container for
holding
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the material and having a dispensing valve provided with a dispensing conduit
or
stem for dispensing the material from the container at the appropriate time, a
syringe
equipped with on/off locking mechanism for permitting or preventing flow of
the
material into and out of the syringe by way of a stem or conduit attached to
the
locking mechanism, and a removable adaptor for connecting the stem of the
syringe
to the stem of the dispensing valve of the pressurized container for
permitting flow of
material from the pressurized container into a chamber of the syringe upon
actuation
of the dispensing valve.
[0005] In a preferred embodiment of the system or apparatus of this invention
the dispensing valve comprises a reciprocatably actuated valve wherein, when
the
syringe stem is connected to the valve stem by way of the adaptor, and the
valve
stem is reciprocatably moved inward towards the interior of the pressurized
container, one or more openings in the valve stem are uncovered permitting
flow of
material from the container to a chamber of the syringe without exposure to
any
contaminants or reactive materials thereby permitting dispensing of the
material
while maintaining its integrity. In another preferred feature of this
invention, a
dessicant is provided for preventing moisture from entering the pressurized
container.
[0006] The invention in one embodiment comprises an apparatus for storing
and dispensing a material from a pressurized container while maintaining the
integrity or purity of the material to be dispensed, the apparatus comprising:
a) a pressurized container holding the material to be dispensed, the
pressurized container having a dispensing valve with a dispensing
valve stem having a distal end protruding from the pressurized
container and a proximal end extending into the pressurized container;
b) a syringe provided with 1) an on/off locking member for permitting/or
preventing flow of the material into or out of a chamber of the syringe
and 2) a stem having an end extending from the syringe for receiving
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material from the pressurized container; and
c) a removable adaptor connecting the distal end of the dispensing valve
stem protruding from the pressurized container to the end of the stem
extending from the syringe so as to establish a permissible flow path
from one stem to the other stem;
so that upon activation of the on/off locking member to the on position,
for permitting flow of material into the syringe and activation of the
dispensing valve to a dispensing mode, material may flow from the
pressurized container to the chamber of the syringe.
[0007] The invention in another embodiment comprises an apparatus wherein
the dispensing valve comprises a reciprocatably actuated valve.
[0008] The invention in another embodiment comprises an apparatus wherein
the valve stem of the dispensing valve is hollow but is closed at the proximal
end in
the container and is provided with one or more covered openings along the
stem,
the valve stem being reciprocatably movable inward into the pressurized
container
for uncovering the one or more openings in the valve stem for permitting the
flow of
material from the pressurized container through the one or more openings, into
the
valve stem, and into the chamber of the syringe.
[0009] The invention in another embodiment comprises apparatus wherein
the one or more openings in the dispensing valve stem are located
circumferentially
around the dispensing valve stem and are covered by a gasket until the
dispensing
valve stem is moved reciprocatably inward into the pressurized container for
uncovering the one or more openings.
[0010] The invention in another embodiment comprises an apparatus wherein
the gasket is a ring of material surrounding the dispensing valve stem in a
slidable
manner.
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[0011] The invention in another embodiment comprises an apparatus wherein
the pressurized container holding the material to be dispensed is a positive
dispense
container comprising a pressurized container having therein a bag containing
the
material to be dispensed, said bag being connected to the dispensing valve in
fluid
flow relationship, and said bag being surrounded by pressurizing gas,
preferably such
as argon or nitrogen, in the container.
[0012] The invention in another embodiment comprises an apparatus wherein
the pressurized container holding the material to be dispensed is a positive
dispense
container comprising a pressurized container having therein a bag containing
the
material to be dispensed, said bag being connected to the dispensing valve in
fluid
flow relationship, and said bag being surrounded by pressurizing gas in the
container. In a further embodiment a desiccant material may be placed in the
space
between the pressurized container and the bag therein holding the material to
be
dispensed, i.e., in the space where the pressurized gas is maintained between
the
wall of container and bag to prevent any moisture in the container from
entering the
bag containing the material to be dispensed.
[0013] The invention in another embodiment comprises an apparatus wherein
the bag is connected to the dispensing valve though a valve connector, the
valve
connector having a central opening for permitting the material to flow out of
the bag,
the dispensing valve stem is seated in the valve connector in a biased manner
in a
direction outwardly from the pressurized container preventing flow of material
out
through the valve stem until actuation of the dispensing valve.
[0014] The invention in another embodiment comprises an apparatus wherein
the dispensing valve stem is seated upon a biasing spring in the valve
connector.
[0015] The invention in another embodiment comprises an apparatus wherein
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the adaptor comprises two female sockets connected by a central material flow
path
passageway in the adaptor, one of the female sockets connected to the distal
end of
the dispensing valve stem and the other female socket connected to the end of
the
stem of the syringe for permitting the flow of the material from the
dispensing valve
stem to the syringe stem so that the material may flow from the pressurized
container to the chamber of the syringe without exposure to the atmosphere.
[0016] The invention in another embodiment comprises an apparatus wherein
the adaptor comprises two female sockets connected by a material flow path,
one of
the female sockets connected to the distal end of the dispensing valve stem
and the
other female socket connected to the end of the stem of the syringe for
permitting
the flow of the material from the dispensing valve stem to the syringe stem so
that
the material may flow from the pressurized container to the chamber of the
syringe.
[0017] The invention in another embodiment comprises an apparatus wherein
the on/off locking member on the syringe is a luer lock.
[0018] The invention in another embodiment comprises an apparatus wherein
the syringe is provided with a reciprocatably actuated piston extending
outwardly
from the chamber of the syringe at an end of the syringe opposite the syringe
stem.
[0019] The invention in another embodiment comprises a method for storing
and dispensing a material from a pressurized container while maintaining the
integrity or purity of the material to be dispensed, the method comprising:
a) providing a pressurized container holding the material to be dispensed,
the pressurized container having a dispensing valve with a dispensing
valve stem having a distal end protruding from the pressurized
container and a proximal end extending into the pressurized container;
b) providing a syringe provided with 1) an on/off locking member for
permitting/or preventing flow of the material into or out of a chamber of
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the syringe and 2) a stem having an end extending from the syringe for
receiving material from the pressurized container; and
c) providing a removable adaptor for connecting the distal end of the
dispensing valve stem protruding from the pressurized container to the
end of the stem extending from the syringe so as to establish a
permissible flow path from one stem to the other stem;
d) connecting the adaptor to the distal end of the dispensing valve stem
protruding from the pressurized container to the end of the stem
extending from the syringe; and
e) activating the on/off locking member to the on position for permitting
flow of material into the syringe;
f) activating the dispensing valve to a dispensing mode permitting
material to flow from the pressurized container to the chamber of the
syringe; and
g) activating the on/off locking member to the off position to isolate the
material in the chamber of the syringe.
[0020] The invention in another embodiment comprises a method having the
additional step of subsequently replacing the stem of the syringe with a
needle,
activating the on/off locking member to the on position and expelling material
from
the syringe chamber to a closed system where the material is to be employed.
[0021] The invention in another embodiment comprises a method wherein the
dispensing valve comprises a reciprocatably actuated valve.
[0022] The invention in another embodiment comprises a method wherein the
valve stem of the dispensing valve is hollow but is closed at the proximal end
in the
container and is provided with one or more covered openings along the stem,
the
valve is actuated by the valve stem being reciprocatably moved inward into the
pressurized container thereby uncovering the one or more openings in the valve
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stem and permitting the flow of material from the pressurized container
through the
one or more openings, into the valve stem, and into the chamber of the
syringe.
[0023] The invention in another embodiment comprises a method wherein the
one or more openings in the dispensing valve stem are located
circumferentially
around the dispensing valve stem and are covered by a slidable gasket and when
the
dispensing valve stem is moved reciprocatable inward into the pressurized
container
the one or more openings is/are uncovered by the gasket to provide for flow of
the
material into the one or more openings.
[0024] The invention in another embodiment comprises a method wherein the
pressurized container holding the material to be dispensed is a positive
dispense
container comprising a pressurized container having therein a bag containing
the
material to be dispensed, said bag being connected to the dispensing valve in
fluid
flow relationship, and said bag being surrounded by pressurizing gas,
preferably
argon or nitrogen, in the container, whereby upon activation of the dispensing
valve
the pressurizing gas forces material from the bag through the dispensing valve
and
into the syringe chamber.
[0025] The invention in another embodiment comprises a method wherein the
bag is connected to the dispensing valve though a valve connector, the valve
connector having a central opening for permitting the material to flow out of
the bag,
the dispensing valve stem is seated in the valve connector in a biased manner
in a
direction outwardly from the pressurized container preventing flow of material
out
through the valve stem until actuation of the dispensing valve occurs.
[0026] The invention in another embodiment comprises a method wherein the
dispensing valve stem is seated upon a biasing spring in the valve connector
and
activation of the dispensing valve causes the biasing spring to be contracted
permitting the dispensing valve stem to further enter the pressurized
container to
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uncover the gasket from the one or more openings circumferentially around the
stem.
[0027] The invention in another embodiment comprises a method wherein the
adaptor comprises two female sockets connected by a central material flow path
passageway in the adaptor, and the adaptor is connected to the two stems by
connecting one of the female sockets to the distal end of the dispensing valve
stem
and the other female socket to the end of the stem of the syringe.
[0028] The invention in another embodiment comprises a method wherein the
material to be dispensed is an ultra dry solvent.
[0030] The invention in another embodiment comprises a method having the
additional steps of subsequently replacing the syringe stem with a needle
while the
locking member is in the off position, and then activating the locking member
to the
on position and expelling material from the syringe chamber to a closed
reactor or
vessel.
[0031] The invention in another embodiment comprises a method wherein the
material is expelled from the syringe chamber by means of a reciprocatable
syringe
piston.
Brief Description of the Drawings
[0032] The invention is illustrated by, but not limited to, the embodiment of
the
invention shown in the figures wherein:
Fig. I is a exploded view, partially in section, of the apparatus or system of
this invention;
Fig. 2 is an enlarged view of a portion of the apparatus or system of Fig. 1;
Fig. 3 is a view of the assembled apparatus or system ready for dispensing
material from the pressurized container;
Fig. 4 is a view of the assembled apparatus or system of Fig. 3, partially
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broken away to show the relative position of the components;
Fig. 5 is an enlarged view of a portion of the assembled apparatus or system
of Figs. 3 and 4, illustrating the activation of the valve to permit flow of
the material
out of the pressurized container; and
Fig. 6 is view illustrating apparatus to illustrate how the material dispensed
into the chamber of the syringe by the apparatus of this invention may be
dispensed
from the syringe.
Detailed Description of the Invention
[0033] The invention is illustrated by, but not limited to, the following
description of preferred embodiments of the invention. As shown particularly
in Figs.
1 and 2, the system or apparatus 10 comprises a pressurized container 12
containing the material, particularly an ultra-dry solvent material, to be
dispensed.
Although any suitable pressurized container can be employed in the apparatus
and
system of this invention, it is preferred to employ a positive dispense
container
having a bag of the material in a container pressurized by a suitable
pressurizing
gas contained in the container but not in the bag. Such positive dispense bags
are
disclosed, for example in US Patent Nos. 5,035,351 5,040,704 5,137,186 and
5,169,037, the disclosures of which are incorporated herein by reference
thereto.
As illustrated in Fig. 1, the pressurized container 12 has a material-
containing bag
14 in which the material 16 is contained. The bag 14 is exteriorally
surrounded by
pressurized gas 18 in the container 12. In an embodiment, any suitable
desiccant
material 58 may be placed in the space between the wall of the pressurized
container 12 and the bag 14, i.e., in the space occupied by the pressurized
gas 18,
to prevent any moisture resident in the container from entering the bag and
contaminating material 16. Any suitable desiccant in any suitable form, e.g.,
powder
or packaged form, may be employed. Preferably the desiccant is a packaged form
and comprises packaged silica gel or molecular sieve desiccant, such as those
available from Sigma-Aldricch, Inc. of St. Louis, MO, as Minipax absorbent
packets
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and from Multisorb Technologies, Inc. of Buffalo, NY as Natrasorb desiccant
packages. The bag 14 containing the material 16 to be dispensed is sealed with
a
dispensing valve assembly 20 by way of a valve connector 22 suitably sealed to
the
bag and having a central opening 24 extending thought the valve connector.
Seated
in the central opening 24 of the valve connector 22 is a reciprocatable
operable
hollow valve stem 26, closed at its inner or bottom proximal end to prevent
flow of
material directly into the proximal end of the valve stem. That closed end of
the
valve stem is located in the portion of the valve connector 22 extending into
the
interior of the container 12 and being seated on a biasing structure 28, such
as a
spring, biasing the distal end of the valve stem outward of the container 12
and
doing so in a mode preventing dispersing of the material 16 from the bag 14.
The
valve stem 26 is provided with one or more circumferentially spaced openings
or
holes 30 at a location along the valve stem within the central opening 24 of
the
valve connector 22 located within the interior of the pressurized container
12.
Dispensing of the material 16 from the container 12 through openings or holes
30 is
prevented by a covering or gasket 32 surrounding the openings or holes when
the
valve stem 26 is outwardly biased as shown in Fig. 1 and 2. The gasket
material 32
may be of any suitable material not detrimental to the material being stored
in the
bag 14. As an example of such a suitable gasket material there may be
mentioned
Gasket CS05-0310-51 from Buckeye Rubber & Packing Co., Cleveland, Ohio. It
will
be understood that the gasket material will be chosen based on its suitability
to the
material 16 to be contained in the bag 14.
[0034] The apparatus or system 10 of the invention further includes an
adaptor 34 having a central passageway 36 through the adaptor and thereby
providing female sockets 38, 40 at each end of the adaptor for receiving a
male
member as explained hereinafter. The adaptor 34 may be of any suitable size or
shape suitable for the intended use and made of any material suitably
compatible
with the material 16 to be dispensed.
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[0035] The apparatus or system 10 of this invention further comprises a
syringe 42 having a central chamber 44 and provided at one end with a
reciprocatably actuated piston member 46 extending outwardly from the chamber
44
in a sealing manner and at the other end a on/off mechanism or locking member
48.
Extending outwardly from the locking member 48 is a hollow stem or conduit 50
for
receiving material 16 from container 12 into syringe chamber 44 and for
dispensing
the material from the syringe chamber into a reactor or reaction vessel. The
locking
member 48 may be a luer lock mechanism or any other suitable on/off mechanism.
The locking member 48, as illustrated in the Figures 1, 3, 4 and 6 has a
turnable
handle 52, that by appropriate positioning either prevents or permits flow of
material
through stem 50 into or out of syringe chamber 44.
[0036] As shown in Figs. 3 and 4, for using the apparatus or system of this
invention, the adaptor 34 is connected to both the valve stem 26 of the
container 12
and to the stem 50 extending from the syringe 42 by placing the male stems
into
sealing arrangement with female sockets 38 and 40, respectively, of the
adaptor.
[0037] When it is desired to dispense material 16 from bag 14 in container 12,
after the syringe stem 50 and container stem 26 are connected by adaptor 34,
downward pressure is exerted against biasing means 28, such as by downward
movement of the syringe 42, such that stem 26 is forced further into central
opening
24 of valve connector 22 as shown if Fig. 5. Gasket 32 remains stationary
against
the upper end 23 of valve connector 22 as the stem 26 moves downward
compressing biasing spring 28 in the central opening 24 thereby exposing the
holes
or openings 30 previously covered by the gasket. Upon uncovering of the holes
or
openings 30, pressurized gas 18 in container 12 causes material 16 to flow out
of
bag 14 and through central opening 24 and then through holes or openings 30
into
hollow stem 26, through the adaptor 34, and then through stem 50 into syringe
chamber 44 upon positioning handle 52 of locking member 48 to the on (open)
position. Once the material is in the syringe chamber 44 the handle 52 of the
locking
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member 48 may be turned to the off (closed) position to isolate the material
16 in the
chamber.
[0038] When it is desired to dispense the material 16 that now resides in the
syringe chamber 44 the syringe stem 50 is removed from female socket 38 of the
adaptor and the stem is replaced with a syringe needle 54 as illustrated in
Fig. 6.
The material 16 may then be dispensed from the syringe chamber 44 by placing
the
needle in a closed reactor or vessel (not shown), turning handle 52 to the on
(open)
position and expelling the desired amount of the material by appropriate
movement
of syringe piston 46.
[0039] The invention is particularly applicable to an apparatus and a method
for dispensing materials that comprises ultra-dry solvents to be dispensed in
relatively small amounts of about 200mL or less, particularly about 100 mL or
less,
and especially amounts of about 10 ml to about 20 mL, under conditions that
require
the integrity and impurity of the material to be maintained and exposure to
atmospheric conditions or other means of contamination are to be avoided.
Examples of such solvent materials include, but are not limited to acetone,
acetonilrile, anhydrous alcohols, bis (2-methoxyethyl)ether, chlorobenzene,
chloroform, cyclohexane, dimethylforamide, dimethyl sulfoxide, ethyl acetate,
ethyl
ether, hexanes, methyl tert-butyl ether, methylene chloride, methyl ethyl
ketone,
tetrahydrofuran, toluene, xylenes and the like
[0040] While the invention has been described herein with reference to the
specific embodiments thereof, it will be appreciated that changes,
modification and
variations can be made without departing from the spirit and scope of the
inventive
concept disclosed herein. Accordingly, it is intended to embrace all such
changes,
modification and variations that fall with the spirit and scope of the
appended claims.
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