U.S. patent number 3,830,369 [Application Number 05/423,794] was granted by the patent office on 1974-08-20 for high pressure gradient chamber for liquid chromatography.
Invention is credited to Ernest H. Pfadenhauer.
United States Patent |
3,830,369 |
Pfadenhauer |
August 20, 1974 |
HIGH PRESSURE GRADIENT CHAMBER FOR LIQUID CHROMATOGRAPHY
Abstract
An element having a chamber therein is secured to a device which
is provided with inlet and outlet passages communicating with the
chamber. A stirrer is positioned in the chamber and serves to mix
liquid within the chamber with a fluid introduced to the chamber
under high pressure via the inlet passage, the resultant mix being
forced out of the chamber through the outlet passage.
Inventors: |
Pfadenhauer; Ernest H. (Costa
Mesa, CA) |
Family
ID: |
23680205 |
Appl.
No.: |
05/423,794 |
Filed: |
December 11, 1973 |
Current U.S.
Class: |
210/198.2 |
Current CPC
Class: |
G01N
30/22 (20130101); G01N 30/34 (20130101); G01N
2030/347 (20130101); G01N 2030/565 (20130101) |
Current International
Class: |
G01N
30/00 (20060101); G01N 30/34 (20060101); G01N
30/22 (20060101); G01N 30/56 (20060101); B01d
015/08 () |
Field of
Search: |
;210/31C,198C
;55/386 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Adee; John
Attorney, Agent or Firm: Cushman, Darby & Cushman
Claims
What is claimed is:
1. A device for developing a high pressure gradient for liquid
chromatography comprising:
a cap;
an element having a chamber therein;
means for securing the element to said cap;
inlet and outlet passages in said cap, said passages communicating
with the chamber; and
stirring means within said chamber for mixing fluid within the
chamber with fluid introduced under pressure to the chamber through
the inlet.
2. A device as set forth in claim 1, wherein said stirring means is
magnetically operable.
3. A device as set forth in claim 1, wherein said cap includes a
recess within which said element is secured.
4. A device as set forth in claim 3, wherein said securing means
comprises a retainer operatively related to the recess and the
element to hold said element within the recess.
5. A device as set forth in claim 3, further comprising sealing
means within said recess engaging the element and the cap to
prevent escape of fluid from the chamber except through the outlet
passage.
6. A device as set forth in claim 1, wherein said element is
provided with a cylindrical cavity to define the chamber, the
device further comprising a stem secured to said cap and projecting
within the cavity, said stem having a passage therethrough
communicating with the inlet passage to introduce the fluid under
pressure to the interior of the chamber.
7. A device as set forth in claim 6, wherein said stirring means is
located between the stem and the bottom of said cavity and is
magnetically operable.
8. A device as set forth in claim 1, further comprising sealing
means engaging the element and the cap to prevent escape of fluid
from the chamber except through the outlet passage.
Description
BACKGROUND AND SUMMARY OF THE INVENTION
Gradient elution is a useful technique in many applications of
chromatography and is particularly applicable to high pressure
liquid chromatography where high resolution and speed of analysis
are obtainable. However, available gradient devices are complex and
expensive. For example, one such device requires a substantial
number of high pressure valves, a holding coil and a gradient
chamber, whereas another known arrangement utilizes a plurality of
pumps to develop the gradient.
The present invention is concerned with a simple, efficient
gradient device which can be produced at a fraction of the cost of
known devices and which permits accurate mixing for a precise
gradient without introducing voids which would interfere with
subsequent detection in the chromatographic column. This is
accomplished by combining an element having a chamber therein and a
cap device. The cap is provided with a suitable passage to direct a
solvent under high pressure into the chamber to be mixed by a
magnetic stirrer with an eluant within the chamber, the pressure
forcing the mix from the chamber through a second passage in the
cap to the liquid column where the analysis is made.
The invention now will be described in greater detail with
reference to the accompanying drawings which illustrate a preferred
embodiment of the invention and wherein:
FIG. 1 is a top plan view of a high pressure gradient chamber
according to the invention;
FIG. 2 is a view partially in section taken along line 2--2 of FIG.
1; and
FIG. 3 is a view in section taken along lines 3--3 of FIG. 2.
Referring to the drawings, the basic components of the device are a
cap 10, element 12, retainer 14, stem 16, and magnetic stirring bar
18. The structural details of these elements can most clearly be
seen in FIGS. 2 and 3.
Cap 10 is a generally cylindrical element. A cylindrical recess 20
is provided at one end of the cap, this recess being threaded along
a portion of its length as indicated at 22. A pair of passages are
machined in the cap, these passages communicating with the recess
20. One of these passages is designated as an inlet passage 24,
while the other passage 26 serves as an outlet. The ends of
passages 24 and 26 remote from the recess 20 communicate with
internally threaded cavities 28 and 30 which receive conventional
fittings 32 and 34, respectively. Fitting 32 is associated with a
conduit 36 which is joined to a source of solvent moved under high
pressure by a pump (not shown), while fitting 34 couples the outlet
passage 26 to a liquid chromatographic column (not shown) via
conduit 38.
Element 12 is generally cylindrical and has an annular flange
portion 40 at one end thereof. The external diameter of the flange
is slightly less than the diameter of the recess 20 in cap 10.
Consequently, element 12 is received within recess 20 as shown. In
order to hold the element within recess 20, retainer 14 is
employed. This retainer is an annularly shaped device having
external threads which cooperate with threads 22 within recess 20.
The diameter of the passage through retainer 14 substantially
corresponds to the diameter of the cylindrical portion of element
12. Consequently, retainer 14 is slipped over the end of element 12
and is screwed into recess 20 so as to engage the shoulders of the
element which are defined by flange 40. Thus, element 12 is held in
position within the recess 20 of cap 10. The retainer 14 is
provided with recesses 42 in one face thereof, these recesses
serving to accept a suitable tool for tightening the threaded
retainer, and thus the element 12 within recess 20.
Element 12 is provided with a central cavity which defines a mixing
chamber 44 and which is co-axial with the cylindrical portion of
the element extending a greater part of the length thereof. The
chamber 44 is of sufficient diameter to communicate with the inlet
and outlet passages 24 and 26. Magnetic stirring bar 18 rests at
the bottom of chamber 44, the bar being a conventional stirring bar
as can be seen more clearly by reference to FIG. 3.
Also located within chamber 44 is stem 16. This stem is generally
cylindrical in shape and is threaded at one end to be received
within a threaded cavity 46 formed at the end of passage 24 in cap
10. A passage 48 extends the length of stem 16 and completes a path
from inlet passage 24 through the stem to the interior of chamber
44.
In order to prevent leakage from the mixing chamber, the upper
surface of flange 40 is provided with an annular groove within
which an O-ring 50 is positioned. This O-ring prevents the passage
of fluid between the mating surfaces of recess 20 and flange 40
when the retainer 14 positions the element 12 within the
recess.
To mount the unit to a suitable support, shown as 52 in FIG. 2, the
cap 10 is provided with a plurality of holes 54 through which
suitable bolts 56 project, the entire assembly being held to
support 52 by nuts 58 secured to the bolts.
The cap, mixing chamber, stem and retainer are preferably made of
stainless steel and O-ring 50 is a material such as polysulfide
which exhibits high solvent resistance.
In operation, the mixing chamber 44 is filled with a starting
eluant and a solvent of high elution power is pumped at high
pressure via conduit 36, inlet passage 24, and passage 48 into the
chamber. Mixing is accomplished by the actuation of stirring bar 18
by means of a magnetic field external to the assembly, the
stainless steel being non-magnetic and therefore not interfering
with the operation of stirrer 18. The high pressure mixture is
forced out of the chamber 44 through passage 26 and conduit 38 to
the chromatographic column.
The actual size of the chamber is determined by the shape of the
gradient desired. The larger the chamber, the less steep is the
gradient developed.
While the device described is particularly adapted to a liquid
chromatography, it also can be used for slurry packing small
packing materials into columns. In such an arrangement, the packing
material is added to a carrier solvent in the desired slurry
consistency and is poured into the mixing chamber. The slurry is
then pumped from the mixing chamber to the column.
* * * * *