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Патент USA US3098728

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July 23, 1963
A. FERRARI
CONCENTRATION APPARATUS FOR QUANTITATIVE
ANALYSIS OF’ A SUBSTANCE IN A LIQUID
3,093,718
Filed Sept. 8, 1959
45
43
INVEN TOR
Arvoges FEQQAW
Arr-owns)’
rates latent O?ficc
Patented July 23, 1963
2
1
a ?uid-tight seal with the mouth of the ?ask.
3,098,718
Hollow
shaft 24 is removably secured by-a chuck St)‘ to the ?ange
CONCENTRATION APPARATUS FOR QUANTITA
TIVE ANALYSES OF A SUBSTANCE IN A LIQUID
Andres Ferrari, Scarsdale, N.Y., assignor to Technicon
Instruments Corporation, Chauncey, N.Y., a corpora
tion of New York
31 of a rotary gear 32 which is journaled in a bearing 33
at the upper end of post 34. An electric motor 35 which
may also be supported on said post ‘a-ctu-ates shaft 24, the
driving connection between the motor and said shaft being
here shown as comprising the bevel gear 36 which meshes
with the bevel gear 32. It will ‘be understood that ?ask
10 may be rotated at a suitable speed, according to the
Filed Sept. 8, 1959, Scr. No. 838,579
6 Claims. (Cl. 23-253)
This invention relates to a liquid concentration and 10 gear ratio of gears 32 and 36 and also by the provision,
treatment method and apparatus. for quantitative analysis
if‘desired, ‘of speed reducing gearing (not shown), driv
of said liquid in respect to a substance therein.
ingly connecting the shaft of motor 35 to shaft 24 in any
suitable way.
One object of the invention is to provide apparatus
A plurality of ?uid passages extend through shaft 24
which is well adapted for use in a continuous analysis
system for ?ash-heating a ?owing stream of a liquid ‘for 15 into ?ask 101. These passages are preferably constituted
by a plurality of glass tubes 38, 401 and 42. Tube 38
partial evaporation thereof, in order to increase the con
provides a tubular passage for the introduction of the
centration of a substance therein, especially inithe case
liquid, which is to be concentrated, into the ?ask at an
of liquids in which the substance is present in ‘minute or
upper part thereof, as clearly shown in FIGS. 1 and 2.
only trace quantities, with concurrent with-dr-awalof the
concentrated liquid and treatment thereof for colorimetric 20 More particularly, the liquid inlet for the ?ask is provided
by the inner end or outlet end 44 of said tube, so that the
examination.
liquid supplied through tube 38 ?ows downwardly on the
In accordance with ‘another object of the invention, the
inner side of the ?ask to the bottom thereof. Since the
apparatus may be provided with means to introduce a
?ask is being rotated and is in heated condition while the
reagent into the liquid under investigation with respect to
a constituent thereof whereby when the liquid containing 25 liquid is introduced into ‘the ?ask, the liquid comes in
contact with successive portions of the ?ask peripherally
said reagent is heated, the constituent which may be pres
ent in a normally insoluble form is. rendered soluble in
the liquid ‘and its concentration therein is increased by
liquid evaporation. For example, in theanalysis of boiler
thereof, as well as longitudinally thereof in the form of a
?lm-like coating on the inner surface of the ?ask so that
rapid evaporation of some of the liquid occurs with con
feed water supplied to steam boilers from condensers in 30 comitant concentration of the liquid during the ?ow of the
liquid to the bottom of the ?ask. Tube 40 provides means
power plants or boiler rooms, such water containing, in
for withdrawing the concentrated liquid from the ?ask
and for this purpose the inner end portion 46 of said tube
is positioned, as illustrated in FIG. ,2, so that it is im
by the addition of sulfuric acid to said liquid andthe heat
ing of the liquid would greatly increase the concentra 35 mersed in the pool of liquid which collects at the bottom
of the ?ask. Tube 42 is provided for withdrawing vapors
tion of the iron whereby to facilitate analysis.
or fumes from the-t?ask'formed as a result of theheating
A further object is the provision of a continuous analy
or ?ash evaporation of some of the liquid which (is ad
sis system or method, as distinguished from a batch or
addition to water-soluble iron, highly oxidized iron which
is considered insoluble, would be rendered totally soluble
mitted through tube 38. Tube 42 is connected to an
discontinuous method of analysis, for performing quanti
tative analyses of a liquid in respect to substances which 40 aspirator 43 of ‘a well known type which is operated by a
stream of water, which ?ows through tube 45‘, for with
are present therein in trace or very small quantities.
drawing the fumes through said tube. The water is also
The above and other objects, features and advantages of
effective to dilute and cool the fumes so that the ?uids
this invention will be fully understood from the following
may be exhausted to waste through the outlet 47. The
description considered in connection with the accompany
ing illustrative drawings.
In the drawings:
' .
.
45 rate of withdrawal of the vapors or fumes may be ad
justed to prevent the accumulation of excessive pressure
within the ?ask.
FIG. 1 is a schematic view illustrative of the apparatus
and method of the present invention;
FIG. 2 is a view partly in elevation and partly in sec
tion and on a larger scale of part of the apparatus; and
FIG. 3 is. a sectional view, on a larger scale, on the line
3-3 of FIG. 2.
tration in ?ask 10, as Well as means for withdrawing from
section can be moved to retracted position to permitthe
insertion and removal of ?ask 10. The electric resistance
heating elements on said sections are indicated at 20, and
it will be understood that the electric heater constituted
spaced relation and which are engaged simultaneously by
The apparatus of the present invention includes means
for transmitting the liquid through tube 38 for concen
the ?ask the concentrated liquid, concurrently with the
introduction into the ?ask of the liquid which is to be
concentrated therein. For these purposes there is pro
Referring to the drawings in detail, the apparatus of
the present invention comprises a glass ?ask 1t} mounted
vided a proportioning pump 52 of any suitable construc
for rotation about its longitudinalaxis and disposed in a 55 tion for transmitting liquids or ?uids into the ?ask and
downwardly inclined position for rotation in said position
withdrawing them from the ?ask at predetermined rates
with an electrically heated oven 12. As illustrated in
of flow. The proportioning pump is preferably of the
FIG. 2, oven 12 has a stationary lower section 14 and an
type described in U.S. Patent No. 2,893,324, issued to
upper movable section 16 which is ‘hinged to the lower
the assignee of the present application. Brie?y described,
section 14 by the hinge indicated at 18 so that said upper 60 said pump comprises a plurality of resiliently compres
sible tubes which are mounted on a platen in laterally
a plurality of pressure rollers which are moved progres
sively along the lengths of the tubes for pumping the
by said resistance elements surrounds the ?ask and also 65 liquids or ?uids therethrough. As the pnoportioning
confronts the bottom thereof ‘as illustrated in FIG. 2.
Sections 14 and 16 of the electrically heated oven 12 are
provided with suitable heat insulation as indicated at 22.
The ?ask lit is mounted for rotation by a hollow rotary
pump does not'in itself constitute a part of the present
shaft 24 which has an end portion 26 which is ?rictionally
described, may be‘emploved solely for the purpose of
concentrating a liquid, for example, when the liquid con
engaged by the mouth 28 of the ?ask, interiorly of the
latter, for removably supporting the ‘?ask and providing
invention, further description and illustration thereof are
unnecessary.
The ‘apparatus of the present invention, as thus far
tains a very small quantity of a substance by reason of
3,098,718
3
4
which quantitative analysis of the liquid in respect to
said substance in the liquid is ordinarily extremely di?'i
through pump tube 66 at the rate of 0.8 ml. per minute.
The liquid introduced into the ?ask is heated to a tem
perature of about 350° C. to 400° C.
While I have shown and described the preferred em
bodiment of my invention, it will be understood that the
cult or impossible, ‘especially in continuous analysis or
monitoring systems. More particularly, in power plant
operations, for example, the analysis of boiler feed water
in respect to the iron or copper content thereof, requires
the employment of trace analysis techniques, such as the
use of long ?ow cell colorimeters and other complicated
devices and procedures because of the low concentration
of iron or copper, as the case may be, in the feed water.
invention may be embodied otherwise than as herein
Accordingly, by treating the boiler feed water ?or in
currently with the performance of the analysis or moni
of this invention within the scope of the appended claims.
What I ‘claim is:
l. Liquid~treatment apparatus, comprising a ?ask
toring operation, the important advantage is obtained by
mounted for rotation about its longitudinal ‘axis, said
creasing the concentration of the iron or copper con
speci?cally illustrated or described, and that certain
changes in the form and arrangement of par-ts and in the
specific manner of practicing the invention may be made
without departing from the underlying idea orprinciples
reason of the factgthat it is possible to employ a contin 15 ?ask ‘being disposed in a downwardly inclined position
uous analysis system without requiring the use of com
during its rotation, means =for rotating said ?ask in said
plicated trace analysis techniques and devices. This will
position about said axis, means ‘for heating said ?ask
be more clearly evident from the following description
during lsaid rotation thereof, and stationary conduit means
of a method of continuous analysis of boiler feed water
extending into said ?ask ‘and providing a plurality of
20 ?uid passages in communication with the interior of the
for the quantitative determination of iron therein.
With further reference to FIG. 1, a stream of the
?ask, said ?ask being rotated ‘about said conduit means
boiler feed water is transmitted by the pump tube 54 to
by said ?ask rotating means, oneiof said passages ter
minating in a liquid inlet positioned above the bottom
a helical glass mixing coil 56 simultaneously with the
of the ?ask ‘adjacent the side thereof so that liquid ad
transmission to said mixing coil of sulfuric acid (50%
concentration) by the pump tube 58. When the water 25 mitted through said inlet flows down and around on the
containing the sulfuric acid is heated to a high tempera * inner heated side of the ?ask during the rotation of said
?ask in contact with successive peripheral portions or
ture in ?ask 10 any iron which may begpresent in the
water and is normally insoluble therein is rendered sol
uble. The ‘acid treated water passes from the mixing
coil 56 to the tube 38 ‘and is introduced by the latter into
the heated revolving ?ask, and as a result any insoluble
iron present in the water is dissolved therein and the total
said inner side to form a liquid ?lm thereon for effecting
a rapid heating and partial evaporation of the liquid as
it flows to the bottom of the ?ask, another of said passages
terminating nearer the bottom ofethe ?ask than said inlet
passage and constituting an outlet passage for the heated
liquid while the ?ask rotates, and another of said passages
iron concentration is increased. The concentrated liquid
having an inlet opening above the termination of said
is withdrawn through the ?ask 10' through the tube 40
and is transmitted through the mixing and cooling coil 35 last mentioned passage and providing an over?ow pas
sage vfor the heated liquid to limit the quantity of con
60 by the pump tube 62 where it is mixed with potassium
thiocy-anate (‘40% concentration) introduced into the
centrated liquid at the bottom of the ?ask while the
mixing coilgby the pump tube 64.
?ask rotates.
Air or other inert
e
a
2. Liquidatreatment apparatus, comprising a ?ask
gas is preferably introduced into the liquid stream prior
to the flow thereof into the mixing coil, through the pump 40 mounted for rotation about its longitudinal ‘axis, said,
?ask being disposed in a downwardly inclined position
tube 66, whereby the stream of liquid is divided by said
during its rotation, means for rotating said ?ask in said
position about said axis, means for heating said ?ask
during said rotation thereof, aid a plurality of stationary
the gas, one of the purposes of segmentizing the stream
being to provide a cleansing action on the tubular pas— 45 conduits extending into said ?ask ‘for providing ‘a plu
rality cf ?uid passages in communication with the interior
sages. The pump tube 62 by which the liquid stream is
of the ?ask, said ?ask being rotated about said conduit
withdrawn from ?ask 10 and transmitted through the
air or other inert gas into ?owing segments of liquid
separated from each other by intervening segments of
means by said ?ask rotating means, one of said passages
terminating in a liquid inlet positioned ‘above the ‘bottom
connected to a tube 68 for transmitting the liquid through
the ?ow cell (not shown) of a colorimeter 7 0‘ which con 50 of the ?ask adjacent the side thereof so that liquid ad
mitted through ‘said inlet ?ows down and around on the
trols the operation of a recorder 72 in a well known
inner heated side of the flask during ‘the rotation of said
manner. It will be understood that the potassium thio
?ask in contact with successive peripheral portions of
cyanite constitutes a color reagent for treating the con
said inner side to form a liquid ?lmrthereon for effecting
centrated liquid stream for colorimetric examination in
respect ‘to the total iron content of the boiler feed water 55 a rapid heating ‘and partial evaporation of the liquid as
it ?ows to the bottom of the ?ask, another of said p'a-‘s
concurrently with the concentration operation.
sages terminating nearer the bottom of the ?ask than
An over?ow tube 74, which is made of glass, is pro
said inlet passage ‘and constituting an outlet pass-age for
vided to limit the quantity of liquid which may collect
the
heated liquid which the ?ask rotates, ‘another of said
in ?ask 10, the inlet end 76 of this over?ow tube being
above the inlet end of tube 46. Said over?ow tube 74 is 60 passages having an inlet opening above the ‘lower end of
said last mentioned passage and providing an over?ow
connected to the aspirator 43 for the removal of excess
passage for the heated liquid to limit the quantity of
liquid from the ?ask, and it will be noted that the stream
heated liquid at the bottom of the ?ask, one of said con
of water which ?ows through the aspirator is effective
duits providing a passage for withdrawing from said ?ask
to cool and dilute the hot liquid.
As an illustrative but not limitative example of the 65 vapors formed during said heating of the liquid.
3. Liquidtreatment apparatus, comprisi?g a ?ask hav
rates of ?ow of the above-mentioned ?uids pursuant to
ing
an open top, an inclined rotary hollow member in
the operation of the proportioning pump 52 concurrently
serted in said open top and engaged therewith for mount
with the continuous concentration described above, it
ing said ?ask for rotation iabout its longitudinal axis in
may ‘be noted that the boiler feed water under analysis 70 a downwardly inclined position, means for rotating said
is transmitted by pump tube 54 at the rate of 11.7 mls.
hollow member ‘and thereby rotating said ?ask in said
per minute, the sulfuric acid is transmitted through pump
position about said axis, means for heating said ?ask
tube 58 at the rate of 1.2 mls. per minute, the potassium
during said rotation thereof, and ‘a plurality of stationary
thiocyanate is transmitted through pump tube 64 at the
conduits disposed in said rotary hollow member and ex-v
rate of 2.0 mls. per minute, and the air is transmitted 75 tending into said ?ask through said open top thereof to
mixing coil together with the potassium thi-ocyanate is
3,098,718
provide a plurality of stationary ?uid passages in com
munication with the interior 10f said ?ask during the
rotation thereof, one of said conduits terminating in a
liquid inlet positioned above the bottom of said ?ask
adjacent the side thereof so that liquid admitted through
said inlet ‘during the rotation of said ?ask ?ows down
and around on the inner heated side of the ?ask during
the rotation of said ?ask in contact with successive pe
ripheral portions of said inner ‘side thereof for effecting
a rapid heating and partial evaporation of the liquid as
it ?ows to the bottom of the ?ask, and another ‘of said
conduits terminating nearer the bottom of said ?ask
than said liquid inlet ‘and constituting an outlet passage
\for the heated liquid.
6
thereon for effecting a rapid evaporation of ‘a portion of
said liquid as it ?ows to the bottom of said vessel, an
outlet tube having its inlet end adjacent the bottom of
said vessel [for withdrawing the heated liquid therefrom
in the form of a stream, said tubes being stationary and
said vessel being rotated around the ‘axes ‘of said tubes
by said rotating means while the ?ask is being heated
and means in liquid ?ow communication with said outlet
tube for treating said withdrawn ‘liquid stream for anal
ysis concurrently with said evaporation operation and
rotation of said vessel.
6. Apparatus for treating a liquid ‘for quantitative anal
ysis in respect to a substance present therein in a small
quantity, comprising a vessel mounted for rotation ‘about
4. Liquid-treatment apparatus, comprising la ?ask hav 15 its longitudinal axis and having a downwardly inclined
inner surface means for rotating said vessel about said
ing an open top, an inclined rotary hollow member in~
axis, means for heating said vessel during its said rotation
serted in said open top ‘and engaged therewith for mount
and thereby heating said inner surface, an inlet tube for
- ing said ?ask for rotation about its longitudinal axis in
said ‘liquid having its outlet end positioned above the
a downwardly inclined position, means for rotating said
bottom of said vessel adjacent said inner surface so that
hollow member and thereby rotating said ?ask in said
liquid admitted through said inlet end ?ows down iand
position about said axis, means ‘for heating said ?ask dur
around said heated inner surface during the rotation of
ing said rotation thereof, and a plurality of stationary
said vessel to form -a liquid ?lm thereon for effecting a
conduits disposed in said rotary hollow member and ex
rapid heating and partial evaporation of the liquid as it
tending into said. ?ask through said open end thereof to
provide -a plurality of stationary ?uid passages in ‘com 25 ?ow-s to the bottom of said vessel, an outlet tube having
its inlet end adjacent the bottom of said vessel for with
munication with the interior of said ?ask while the ?ask
drawing the concentrated liquid therefrom in the form
rotates, one of said conduits terminating in ‘a liquid inlet
of a stream, said tubes being stationary and said vessel
positioned above the bottom of said ?ask adjacent the
being rotated around the axes of said tubes by said ro
side thereof so that ‘liquid admitted through said inlet
?ows down and around on the inner heated side of the 30 tating means while the ?ask is being heated, means in
liquid ?ow communication with said outlet tube for treat
?ask during the rotation of said ?ask in contact with
ing said withdrawn liquid stream for analysis concur
successive peripheral portions of said inner side thereof
rently with said evaporation ‘operation and rotation of
for effecting ‘a rapid heating and partial evaporation of
said vessel, and a stationary tube extending into said
the liquid as it ?ows to the bottom of the ?ask, another
of said conduits terminating nearer the bottom of said 35 vessel to a point above end of said ‘outlet tube for With
drawing vapors formed during the heating of said vessel.
?ask than said liquid inlet and constituting an outlet
passage for the heated liquid, and another of said con
References Cited in the ?le of this patent
duits having an inlet opening ‘above the lower end of
said last mentioned conduit for providing ‘an ‘over?ow
UNITED STATES PATENTS
passage for the heated liquid to limit the quantity of
1,086,432
Zinkeiser et a1. ________ __ July 14, 1911
liquid in said ?ask.
1,231,247
Freeman ____________ __ June 26, 1917
5. Apparatus for treating a liquid for quantitative anal
ysis in respect to a substance present therein in ‘a small
quantity, comprising a vessel mounted for rotation about
its ‘longitudinal axis and having ‘a downwardly inclined 45
inner surface means for rotating said vessel about said
axis, means for heating said vessel while it is being ro
2,686,754
2,879,141
2,899,280
2,941,501
Monod _____________ __ Aug.
Skeggs _____________ __ Mar.
Whitehead ___________ __ Aug.
Bell ________________ __ June
17,
24,
11,
21,
1954
1959
1959
1960
OTHER REFERENCES
tated about said axis, an inlet tube for said liquid having
Analytical
Chemistry,
volume 14, Feb. 15, 1942, page
its outlet end positioned ‘above the bottom of said vessel
adjacent said inner turface- so that liquid admitted through 50 166, “Determination of Solubilities of Gases at High
Temperatures and High Pressures by the Rotating Born ,”
said inlet end ?ows down ‘and 'around said inner surface
by Ispatieff et a1.
during the rotation of said vessel to form a liquid ?lm
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