U.S. patent number 3,923,464 [Application Number 05/291,763] was granted by the patent office on 1975-12-02 for combustion apparatus for analytical instruments.
This patent grant is currently assigned to Leco Corporation. Invention is credited to Robert N. Revesz, George J. Sitek.
United States Patent |
3,923,464 |
Sitek , et al. |
December 2, 1975 |
Combustion apparatus for analytical instruments
Abstract
A combustion furnace for analytical apparatus in which the
products of combustion of samples are to be transported in a gas
stream for analysis wherein the admission of carrier gas is
separate from the admission of combustion gas, resulting in a
reduction of eddy currents of the gases within the furnace, so
leading to a faster transfer of the component to be measured and to
reduced purge and combustion time.
Inventors: |
Sitek; George J. (Stevensville,
MI), Revesz; Robert N. (St. Joseph, MI) |
Assignee: |
Leco Corporation (St. Joseph,
MI)
|
Family
ID: |
23121726 |
Appl.
No.: |
05/291,763 |
Filed: |
September 25, 1972 |
Current U.S.
Class: |
422/78;
138/40 |
Current CPC
Class: |
G01N
31/12 (20130101) |
Current International
Class: |
G01N
31/12 (20060101); G01N 031/12 (); F15D
001/00 () |
Field of
Search: |
;23/23PC,253PC,292
;219/10.43 ;55/386 ;73/61.1C ;210/198C ;161/125,139,206
;138/40,89,109,174 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Wolk; Morris O.
Assistant Examiner: Turk; Arnold
Attorney, Agent or Firm: Price, Heneveld, Huizenga &
Cooper
Claims
We claim:
1. A combustion furnace for analytical apparatus comprising an
induction coil with a vertically extending axis, a combustion tube
mounted within said coil, an upper closure member for sealably
coupling to an upper end of said combustion tube, said upper
closure member including an exhaust gas passage therethrough, and a
separate aperture extending through said upper closure member along
the vertical axis thereof, a lower closure member for sealably
engaging the lower end of said combustion tube, said lower closure
member including a passageway extending therethrough to define a
carrier gas inlet communicating with the interior of said
combustion tube and crucible supporting means associated with said
lower closure member, said lower closure member movable between a
first position sealing said lower end of said combustion tube and
supporting a crucible within the field of said coil and a second
position displaced therefrom, a combustion gas lance, and means in
said upper closure members for securing said lance in said separate
aperture for optimal delivery of combustion gas into said crucible
within said field.
2. The combination as claimed in claim 1 wherein said exhaust gas
passage of said upper closure member extends vertically through a
bottom surface of said upper closure member to communicate with the
interior of said combustion tube and includes a radially extending
portion extending through a side of said upper closure member for
providing an exhaust port for removal of combustion gases from said
combustion tube.
3. The combination as claimed in claim 2 wherein said upper closure
member includes a sealing member extending around the exterior of
the lower periphery thereof to engage an inner surface of said
combustion tube for sealing said upper closure member to said
combustion tube.
4. The combination as claimed in claim 3 wherein said combustion
tube is a cylindrical sleeve having a circumferential constriction
formed at its upper end and immediately below said sealing member
and extending inwardly sufficiently to shield said sealing member
from combustion by-products.
5. A combustion furnace for analytical apparatus comprising an
induction coil with a vertical axis, a vertical combustion tube
within said coil, a base closure member mounted against the bottom
end of said tube and having passage defining means for delivering
gas into said tube, a vertically reciprocable elevator movable
between a position of sealing against said base member and
supporting a crucible within the field of said coil and a position
downwardly displaced therefrom, a top fitting closing the top end
of said combustion tube, means defining a second gas passage
therethrough, and an oxygen lance mounted in said top fitting for
delivering combustion gas into said crucible.
6. The combination as claimed in claim 5 wherein said oxygen lance
is adjustably mounted in said top fitting for adjustment toward and
away from said crucible.
7. The combination as claimed in claim 5 wherein said lance is a
high silica tube and said top fitting telescopes within the top end
of said combustion tube, said top fitting having a sealing ring
thereabout in the telescoped portion thereof to seal against the
interior surface of said combustion tube, said tube having a
circumferential constriction extending inwardly immediately below
said top fitting a distance sufficient for shielding said sealing
ring from combustion by-products.
8. For use in a furnace for heating specimens to their combustion
temperature wherein the specimens are placed in a crucible
positioned in a combustion tube with sealed end closures, and means
extending through the end closures to provide a flow of gas through
the combustion tube to carry combustion gases from the combustion
tube, an improved combustion tube comprising:
a continuously extending cylindrical body having a first open end
the interior wall surface of which defines an interior cylindrical
sealing surface immediately adjacent said first open end and a
circumferential restriction formed inwardly in said cylindrical
body and spaced from said first end to shield said sealing surface
from combustion by-products, said combustion tube including an
enlarged open opposite end defining a cylindrical wall extending
substantially parallel with said cylindrical body and defining a
cylindrical interior sealing surface having a diameter greater than
the diameter of said cylindrical body.
9. The combustion tube as defined in claim 8 wherein said
combustion tube is made of high silica glass.
10. An induction furnace comprising:
a vertically extending induction coil;
a cylindrical combustion tube positioned within said induction coil
and including an open upper end, an enlarged cylindrical lower open
end and a circumferential restriction spaced from said open upper
end;
an upper closure member for sealably fitting into said upper end of
said combustion tube and including an axial opening through an end
thereof for receiving an oxygen lance tube therethrough and further
including a relatively large opening formed axially upwardly
through a bottom surface of said upper closure member and
communicating with a radially extending port for exhausting
combustion and carrier gases from said combustion tube, said upper
closure member including a peripheral sealing member positioned
adjacent said restriction of said combustion tube; and
a lower closure member including means for supporting a crucible
within the induction field of said induction coil when said lower
closure member is sealably fitted in the enlarged lower end of said
combustion tube, said lower closure member including an axially
extending aperture opening at the top surface of said lower closure
member and means for introducing a carrier gas to said last named
aperture to provide a flow of gas upwardly through said combustion
tube.
Description
BACKGROUND OF THE INVENTION
In U.S. Pat. No. 2,809,100 dated Oct. 8, 1957, to G. J. Krasl,
entitled "Combustion Analyzer", there is shown a glass capsule
adapted to fit within an induction coil and to fit over a crucible
supported on a post which positions the crucible within the field
of the combustion coil. The bottom of the capsule is open for the
vertical elevation of the crucible and post thereinto and is closed
by a base plate carrying the post brought up into contact with the
bottom of the capsule. The base plate has a passage therethrough
for the downward flow of exhaust gases from the capsule. A tube
extends centrally down through the top of the capsule into a
position to direct a jet of oxygen into the crucible when it is in
its elevated position. In use, a sample in a crucible is elevated
into the capsule and heated by the induction coil. At the same
time, oxygen is directed down onto the sample to support its
combustion and the products of combustion together with a carrier
stream of excess oxygen from the jet are carried out through the
bottom of the capsule for electronic analysis.
This apparatus does not function as well as it might for several
reasons. There is a dead space above the crucible between the jet
tube and the wall of the capsule in which eddy currents will exist,
delaying the total transfer of the material to be analyzed and
leading to a trailing of the combustion gases which causes a
tailing of the analysis curve. Optimum readout is derived from a
total transfer of the product to be analyzed within as short a time
period as possible, or in other words, an abrupt rise in the
transfer curve to a high peak and an abrupt decline or decay
thereafter. Eddying of the carrier gas extends the rise time,
reduces the peak, and causes the decay curve to tail off gradually.
The same eddy currents cause a depositing of metal on the walls of
the capsule which, in time, couple to the field of the induction
furnace and destroy the capsule.
By virtue of the single inlet port for the gas which serves both a
combustion and carrier function which is directed straight into the
crucible, the velocity of gas flow is desirably limited to avoid
excessive reaction temperatures and excessive turbulence. Under
conditions of a high content of combustible material, the
combustion process can absorb the whole input of combustion gas and
create a below-atmospheric pressure condition within the capsule.
This necessarily extends the analysis time because the
transportation of the unknown must await the completion of the
combustion. Furthermore, in analytical procedures involving such
sensors as conductivity cells in bridge configurations, it is
necessary to have a constant flow of gas through the cell because
these measurements are flow sensitive. The total absorption of the
gas during combustion results in a flow change or even a backflow
of the gas stream.
SUMMARY OF THE INVENTION
The present invention is directed to a combustion apparatus lacking
blind corners or ends wherein eddy currents might develop. The
apparatus is characterized by two gas inlet ports, one intended
essentially for combustion and the second intended essentially for
transport whereby a continuous flow may be obtained through the
apparatus. By operating the device above ambient pressure, the
combustion process only decreases the pressure and a constant flow
still exists to satisfy the measurement criteria. The device
likewise includes provision for positioning the combustion gas
inlet whereby optimum combustion circumstances can be provided. The
device may operate continuously above or below ambient pressure if
constant flow is not necessary. The device is easily cleaned and
therefore less subject to damage from sculling, and the
destructible element of the combination, the jacket, is inexpensive
and easily replaced. Other advantages of this invention will appear
in the course of the description which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a central vertical section through an induction furnace
embodying the present invention.
DESCRIPTION OF A PREFERRED EMBODIMENT
The furnace 10 consists of a stationary furnace proper 11 and a
vertically reciprocable crucible elevator 12. The stationary
furnace 11 includes a base 13 which consists of a flat, annular
plate 14 having upper and lower flanges 16 and 18 about the central
aperture 20 thereof. The upper flange is externally grooved for the
reception of an O-ring 22. The under side of the plate also has a
downwardly extending outer flange 24 thereabout which likewise is
grooved on its exterior surface for the reception of an O-ring 26.
A carrier gas inlet tube 28 opens into and extends from the central
aperture 20 through the lower flanges 18 and 24 and terminates in a
free end 30 well beyond the plate 14 and the confines of the
furnace itself.
A Vycor.sup.R or similar high silica glass or fused silica
combustion tube 32 is mounted on the base 13. The combustion tube
is of relatively large diameter so as to contain comfortably the
crucible 34 leaving ample gas flow space thereabout. The tube fits
in spaced relation within the induction coil 36. The tube is belled
out at its lower end 38 to fit over the upper flange 16 of the base
13 to rest on its bottom edge against the annular plate 14 and to
engage the O-ring 22 in sealed relation. Adjacent its upper end 40,
the tube has a circumferential restriction 42 therein for purposes
to be described later.
The tube mounts at its upper end a top fitting 44. This top fitting
is a generally cylindrical member with a side arm 46 and an
integral flange 48 thereabout below the side arm 46. The fitting is
externally grooved below the flange 48 for the reception of an
O-ring 49. A large diameter central bore 50 extends from the bottom
of the fitting upwardly to a point adjacent the top of the fitting,
and the side arm 46 has a bore 52 therein intersecting the axial
bore 50. The axial bore 50 terminates at an upper transverse wall
54 having a small diameter axial passage 56 therethrough. A
threaded hole 58 extends from the top end of the top fitting down
to the wall 54. A combustion gas adaptor 60 is threaded into the
hole 58. The adapter 60 is a simple tubular member having exterior
threads at its lower end for engagement with the threaded bore 58
and a central longitudinal passage 62 therethrough and internally
threaded as at 64 at its upper end for the reception of an oxygen
supply fitting (not shown).
The internal bore 62 loosely receives a length of quartz tubing 66
constituting an oxygen lance. The tubing has an annular rubber
bushing 68 fitted on the exterior thereof. The bushing is slidable
along the tubing for adjustment of the lance position. The bushing
is adjusted on the lance to obtain a proper positioning of the
lance for optimum performance with respect to the crucible 34, and
the combustion gas adaptor is screwed down on the bushing 68 to
compress it against the wall 54 and bulge it against the lance 66
to effect a seal and hold the lance securely.
The elevator 12 is mounted on the top end of a vertically
reciprocable rod 70. The elevating mechanism may be identical with
that described in the above-mentioned patent to Krasl. The elevator
consists of a shallow dish 72 having a rim 74 with a vertical
inside wall 76 beveled at its top edge proportioned to telescope
over the outer flange 24 of the furnace base 13 in sealing relation
with the O-ring 26. The dish may have a central internally threaded
downward sleeve 78 whereby the dish is mounted to the post 70 and
an internally threaded central sleeve 80 extending upward from the
floor of the dish 72. The sleeve 80 receives a stud 82 having a
lower threaded end 84, a hexhead 86, and a cylindrical plug 88
upward of the head 86. A tubular ceramic crucible support is
carried on the plug 88 and mounts the crucible 34 at its upper end.
The adjustment capability of the stud 82 is, of course, to position
the crucible optimally within the induction coil 36.
The plate 14 of the base 13 and the flange 48 of top fitting 44 may
be perforated as at 90 for the attachment of the furnace to
brackets 92 whereby the furnace may be mounted to a cabinet or
other element of the analytical apparatus.
From the foregoing, it will be appreciated that the assigned
advantages of this invention have been well met. The provision for
two gas inlets makes possible the continuous purge, avoidance of
dead spaces, and avoidance of below-ambient pressure with
combustion. The provision of the gas passages in the end fittings
makes possible a low cost, simple tube and provides for a direct
end-to-end passage of the gas. Gas flow through the apparatus may
be continuous, and this immediate transfer, together with reduced
purge time, appreciably shortens analysis time.
The upward flow of heated gases from the sample combustion, in the
absence of the constriction 42 in the tube 32, exposes the O-ring
49 to excessive temperatures and hot dust due to the direction of
flow of the exhaust stream, subjecting it to damage and possible
failure, which, of course, cannot be tolerated as leading to
erroneous results. It has been found that the constriction 42
effectually shields the O-ring seal from damage by screening the
seal from radiation from the burning sample and by deflecting the
hot carrier gas stream with entrained products of combustion into
the top fitting 44.
* * * * *