CONTROL OF LABORATORY EVAPORATION

Abstract: Apparatus for evaporating liquid to obtain solid residue. The invention is particularly useful where small quantities of a solid are to be recovered from a first liquid medium (14) and dissolved in another liquid medium. The invention comprises a receptacle (12) for holding the liquid (14) to be treated and flow directing apparatus (24) to localize transport of an evaporating or carrier gas along the wall of the receptacle as it moves downwardly and into contact with the material to be treated. Such localization of inlet gas also provides a relatively quiescent central zone (32) in the receptacle through which the gas, carrying evaporated liquid, can be removed without disturbing the flow of inlet gas. Apparatus (76, 60) to sense the temperature of the evaporating process and terminate the process at any appropriate temperature conditions is provided.

Description: CONTROL OF LABORATORY EVAPORATION BACKGROUND OF THE INVENTION This invention relates to (a) novel processes for controlling the evaporating of liquid from a chemical sample, with drying gas, or like processes, and (b) apparatus useful in such processes. It is often desirable to transfer a solute from one solvent system to another solvent system. For example, this procedure is used frequently in liquid chro atography where a first solution, perhaps a liquid fraction obtained from one chromatographic pro¬ cedure, can be more specifically analyzed by use of a different solvent to carry the dissolved components of the first solution. In the past, it has been common to place the first solution into a tube and, using a gas sparge tube, or cannula, contact the solution with sufficient drying gas to remove the unwanted liquid. Sometimes, too, a sensitive solid product is damaged by continuing to pass drying gas into the apparatus beyond the optimum drying point. Moreover, it is sometimes desirable to leave the solid contents in a somewhat pasty or damp condition. At present, to avoid damage of such samples, it is convenient to dry stepwise or to slow down the drying rate to a fraction of the possible drying rate, thereby reducing the chance that an operator will be inattentive for a period long enough to allow the samples to be dried excessively. SUMMARY OF THE INVENTION It is a principal object of the invention to pro¬ vide a novel process whereby laboratory evaporation procedures are made more efficient by an improvement in the means by which the appropriate dryness of a sample, or any appropriate end-point for -an evapora¬ tion process, is achieved. It is a further object of the invention to pro- vide a novel process whereby dried samples of predic¬ table rewettability or dryness may be provided rapidly. Another object of the invention is to provide a superior process, and improved apparatus, for moni- toring the quality of solids being prepared by eva¬ porative process. It is a further object of the invention to pro¬ vide novel process whereby dried samples of excellent uniformity are provided rapidly. Another object of the invention is to provide a superior process, and improved apparatus, for moni¬ toring the quality of off-gases from a gas-purged vessel. Still another object of the invention is to segregate, and thereby facilitate, the disposal of incoming drying gas from the gaseous effluent leaving c-i evaporator. Other objects will be obvious to those skilled in the art on their reading of this application. The above objects have been substantailly achieved by construction of a sample-processing system comprising a receptacle for liquid being processed and gas feed means to supply carrier gas into the recep¬ tacle such that the gas follows a path downwardly along the receptacle wall until it reaches the material to be treated. This procedure serves to leave a relatively free central path in the receptacle through which the process gas, now laden with any material being evaporated, may proceed upwardly through the central portion of the volume enclosed by the walls of the receptacle. Because the gas leaving the receptacle is not much diluted by mixing with the incoming gas, it is more sensitive to analysis by any number of procedures. For example, it may be ther¬ mally evaluated for the "end point" of an evaporation step. It is important to understand that this end point can be characterized by an absolute temperature, a temperature differential, or a rate in change of temperature. The incoming gas port is sufficiently remote from the material being dried that it does not cause any significant mixing but merely provides a stream of gas moving across the mateial to be dried. Thus one particularly advantageous analytical procedure, facilitated by the construction and opera¬ tion of that part of the invention described above, is the use of a collection tube for removing the outgoing gases and mounting, on it or in it, a thermister for sensing the temperature of the offgas. Such a device, on sensing a rise in temperature of the offgas, would report the completion, or near completion, of the drying to a control means which would respond with an appropriate action. For example, it could shut off the drying gas, alarm an operator, or the like. Another important advantage of the invention is that the advantageous helical flow pattern - charac- terized by a rapid flow of gas across the surface of the liquid being evaporated - remains even over very substantial changes in the height of the liquid being processed within the tube. In one advantageous mode of the invention, the receptacle will be tubular and will be equipped with a tube for supplying incoming gas. This outlet of the gas-supply tube will be so arranged that it will pro¬ vide a generally helical flow path along the interior wall of the tube until it reaches the material being treated. Thereupon, the outgoing gas will rise and exit a central outlet port which may be conveniently tied to an exhaust manifold. In practice, it is contemplated that a number of such evaporating units will share a single laboratory station. Each unit can, typically, consist of a drying tube, a closure means for the drying tube which would also forms means to hold and position the inlet and outlet gas conduits. Each drying tube would be held in a thermostated stand and the closure members with the inlet and outlet conduit could be con¬ veniently positioned on the stand also. While the subject invention will probably be most 5. ' useful in evaporative processes wherein a solid resi¬ due is left behind, it should be.,noted that it has a number of other uses. It could be used very effec¬ tively to sublimate solids from a mixture being treated. Such sublimation processes could use 0 incoming gases of appropriate temperatures. It also is used very effectively to evaporate films of the top layer of non-miscible liquids in the tube. Finally, it could be used as a short-term gas-purge device, for example where nitrogen or- argon might be used over a 5 short period of time to preserve samples of a chemical before subsequent processing. In each case the assurance that the inlet flow would be effectively conducted to the material being treated would be an important advantage. 0 However, it is also useful to sense the tem¬ perature or rate of temperature change at the site of evaporation near the bottom of the drying tube. This can be accomplished by the use of sensors inside the tube, buried in the tube wall, or outside the tube. 5 Moreover, the temperature could be sensed by the temperature-sensitive robot hands constructed according to the principles described in the article "A Simple Thermal Touch Sensor" appearing in Vol. 6, No. 10 of Robotics Age magazine R.A. Russell, which 0 article is herein incorporated by reference. It also should be noted that the apparatus, as illustrated below, is particularly useful in conjunc¬ tion with robot means. A robot arm can be used to pick up a conduit-bearing closure from a storage shelf and place it into the test tube. Moreover, as indi¬ cated above, the temperature-sensing element may be associated directly with a robot hand which carries said tube. ILLUSTRATIVE EMODIMENT OF THE INVENTION In this application and accompanying drawings there is shown and described a preferred emodiment of the invention and suggested various alternatives and modifications thereof, but it is to be understood that these are not intended to be exhaustive and that other changes and modifications can be made within the scope of the invention. These suggestions herein are selected and included for the purposes of illustration in order that others skilled in the art will more fully understand the invention and the principles thereof and will be able to modify it and embody it in a variety of forms, each as may be best suited to the condition of a particular case. IN THE DRAWINGS Figure 1 is a perspective view, somewhat schema- tic, of an apparatus constructed according to the invention. Figure 2 is a view downwardly of one apparatus according to the invention showing the position of a gas inlet conduit. Figure 3 is a perspective view, somewhat schema- tic, of a station comprising a number of apparatus described in Figure 1. Figure 4 shows relative position between a gas inlet conduit and a temperature-sensing means. Figure 5 is a control circuit useful with the apparatus and process of the invention. Referring to figures 1 and 2, it is seen that the liquid-evaporating apparatus 10 comprise a test tube 12 forms a vessel for receiving a quantity of liquid 14 which comprises a solute dissolved therein. Tube 12 is equipped with a closure 16 through which gas inlet conduits 18 and gas inlet 20 pass into the headspace 22 within tube 12 and above liquid 14. Conduit 18, about 0.030 inches in inside diameter is arranged such that its terminal portion 24, and its discharge port 26 cause the gas to be discharged somewhat downwardly (preferably at an angle of from 10 to 50 angular degrees, but most advantageously at about 15 to 30 degrees) along the interior wall 28 of tube 12. As indicated schematically at 30, the gas flow from conduit 18 hugs the wall in a helical pat¬ tern until it reaches liquid 14 (or wet solid which gradually appears as its solvent is evaporated from the mass of liquid 14). The motion of the inflowing gas induces a natural internal path for removal of moisture-carrying gas up the central portion of the test tube, as indicated at 32 of Figure 1. Thus, the incoming and outgoing gai ■ are maintained in a very useful degree of segregation. The gas is carried past a thermister 60 which forms means for sensing the temperature of the gas and reporting such temperature to circuitry which, in response to said temperature, stops or controls the flow of drying gas. Figure 3 illustrates one convenient way to uti¬ lize the invention. Several of the apparatus 10 are utilized in conjunction with a central processing sta¬ tion 40. The closures 16 are kept on a shelf 42 with the necessary flexible conduits 18a and 20a extending, retracted, behind the facade 44 to manifolds 46 and 48 respectively. The test tube holding receptors 50 in station 40 are desirably ther ostated electrically in a "dry" heat bath, e.g. an aluminum block. Figure 4 illustrates an apparatus 70 how a tem¬ perature sensor 72 can be positioned in a test but 74 to the sample being treated. The sensor 72 sits on an insulating gasket 7 and is operably connected to a control sensing circuit by electrical conduit 78. This is often preferred when more sensitive tem¬ perature measurements, e.g. detection of a mere slowing of the rate of evaporation is desirable. Figure 5 illustrates a schematic diagram of a simple control circuit 80 useful with the invention. Circuit 80 comprising a thermal sensor 82 having a voltage output proportional to the temperature of the material being dried. The signal is buffered as through an amplifier/filter system 84 and then the resulting signal is compared in a comparitor 86 against a set point, e.g. as with variable resister 88. The resulting signal is usually further processed according to the needs of a particular system through an amplification system and the output signal is used to control a drying-gas cooling supply as by operation of a solenoid valve as indicated at 92, or to actuate an alarm to alert an operator, or to vary the rate of drying gas, etc. Such sensitive measurements make it easy to detect and stop a drying action by cutting off the supply of drying gas when a solid residue is still wet and susceptible to easy redispersal and solvation. Also, it provides a means to assure sensitive biologi¬ cal products are not damaged by excessive drying. It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described and all statements of the scope of the invention which might be said to fall therebetween.

Claims: AMENDED CLAIMS [received by the International Bureau on 03 February 1987 (03.02.87); original claims 1—13 replaced by amended claims 1—16 (5 pages)] 1) A process for recovering solids from liquids by evaporating said liquid until said solids have been converted to a solid composition of a desired state of dryness, said process comprising the steps of: (a) placing a liquid composition containing said solids and said liquid in a tubular receptacle; (b) causing drying gas to flow into said recep-≤ tacle through an inlet to said tubular receptacle which inlet directs the flow of said drying gas preferentially along the wall of said receptacle • and into intimate contact with said solution as the liquid is being removed form said solution; (c) then removing said drying gas through another conduit in said inlet of said tubular receptacle while avoiding dilution of said gas by said incoming gas so as to maintain a significant te - perature difference between incoming drying gas and outgoing gas during said evaporating process; (d) sensing a change in rate of evaporation by thermally monitoring the temperature of said eva- poration process; and (e) decreasing the flow of drying gas in response to said sensed change in rate of evaporation, thereby obtaining said solid in said desired state. 2) A process as defined in Claim 1 and wherein said incoming gas is directed in a -helical path from a position proximate the top of said container along the interior wall of the container to contact said liquid being evaporated, and wherein said outgoing gas is pre- ferentially reir ved upwardly through the central region of said container. .5 5 3) A process as defined in Claim 2 wherein said tem- perature of said drying gas is sensed as it is being removed from said receptacle and is used as a criterion for determining said desired rate. 4) A process as defined in Claim 2 wherein said heli- cal path is initiated at an angle of from about 10 to 50 angular degrees downwardly from hori__ontal. 5) A process as defined in Claim 1 wherein the tem- perature of the material being dried is sensed, at a posi- tion proximate to said material, and used as a criterion of said desired state. 6) Apparatus for isolating solids from liquids by evaporating said liquid, said apparatus comprising: (a) a tubular vessel having a closure only at the top thereof and forming means to hold a liquid composition position to be dried to a suitably dry state near the bottom thereof; (b) a first supply conduit through said closure and positioned near the top of said vessel forming means for conveying drying gas into said tube through said opening, and into contact with said composition being dried; (c) a second conduit located in said closure and forming means to remove said drying gas after it has contacted said composition being dried; (d) each said conduit means accessing said tube at said tubular opening and said conduits together forming a means to avoid excessive dilution of incoming gas by gas being removed from said vessel; (e) a control circuit forming means to sense a tem- perature condition of said evaporating; and (f) circuit means to reduce or stop the flow of said drying gas in response to said temperature condition. i o 7 ) Apparatus as defined in Claim 6 wherein said first supply conduit forms means to direct said incoming gas in a helical path along the interior wall of said tube and wherein said second conduit is centrally located within said single opening. 8) Apparatus as defined in Claim 7 wherein said tubu- lar vessel is a test tube. 9) Apparatus as defined in Claim 8 wherein said tubu- lar vessel is a test tube. 10) Apparatus as defined in Claim 8 wherein said first supply conduit forms means to direct said incoming gas in a helical path at an angle of from about 15 to 30 angular degrees downwardly along said wall. 17 11) A process for recovering solids from liquids by evaporating said liquid by evaporating said liquid until said solids have been converted to a solid composition of a desired state of dryness, said process comprising the steps of: (a) placing a liquid composition containing said solids and said liquid ".n a tubular receptacle; (b) causing drying gas to flow into said receptacle through an inlet to said tubular receptacle which inlet directs the flow of said drying gas in a generally helical flow pattern from a position in said tubular receptacle which is remote from said liquid composition around and downwardly along the wall of said tubular receptacle and thence into intimate con- tact with said liquid composition, to remove moisture therefrom; and (c) then removing moisture-bearing drying gas through an internal path, generally within said helical flow gas pattern of said "incoming drying gas, and through an outlet conduit positioned at the axis of said heli- cal flow pattern and near the top of said tubular receptacle, thereby avoiding dilution of said moisture-bearing drying gas being removed by said incoming drying gas and maintaining a significant temperature difference between the incoming drying gas and the moisture-bearing drying gas being removed during said evaporating process. 12) A process as defined in Claim 11 wherein said helical flow pattern is initiated at an angle of from about 10 to 50 angular degrees downwardly from horizontal. 13) A process as defined in Claim 12 wherein said helical flow pattern is initiated at an angle of from about 15 to 30 degrees downward from horizontal. 14) Apparatus for isolating solids from liquids by evaporating said liquid, said apparatus comprising: (a) a tubular vessel having an opening only at the top thereof and forming means to hold a liquid composition to be dried to a suitably dry state near the bottom thereof; (b) a closure, -jneans closing said opening; (c) a first supply conduit means through said closure means and positioned near the top of said vessel for conveying drying gas through said opening into said tubular vessel in a helical path along the interior wall thereof, and into contact with said composition being dried; (d) a second conduit means located in said closure means at a location on the axis of said helical path to remove said drying gas after it has contacted said composition being dried; and (e) each said conduit means accessing said tubular vessel at said opening thereby together forming a means to avoid excessive dilution of incoming gas by gas being removed from said vessel. 15) Apparatus as defined in Claim 14 wherein said tubular vessel is a test tube. 16) Apparatus as defined in Claim 14 wherein said first supply conduit means directs said incoming gas in a helical path at an angle of from about 15 to 30 angular degrees downwardly along said wall.

Inventors: FRISWELL DAVID R, FRISWELL, DAVID, R.
Applicants: ZYMARK CORP, ZYMARK CORPORATION
Application year: 1986
Main classification: B01D1
IPC codes: B01D1