US3219416A - Apparatus for the automatic chemical sequential treatment and analysis of small quantities of material - Google Patents

Apparatus for the automatic chemical sequential treatment and analysis of small quantities of material Download PDF

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US3219416A
US3219416A US23401962A US3219416A US 3219416 A US3219416 A US 3219416A US 23401962 A US23401962 A US 23401962A US 3219416 A US3219416 A US 3219416A
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means
capillary tube
dispensing
capillary
tube
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Natelson Samuel
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Scientific Ind Inc
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/025Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations having a carousel or turntable for reaction cells or cuvettes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00178Special arrangements of analysers
    • G01N2035/00237Handling microquantities of analyte, e.g. microvalves, capillary networks
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices

Description

5. NATELSON Nov. 23, 1965 APPARATUS FOR THE AUTOMATIC CHEMICAL SEQUENTIAL TREATMENT AND ANALYSIS OF SMALL QUANTITIES OF MATERIAL Filed Oct. 30, 1962 3 Sheets-Sheet 1 INVENTOR SAMUEL NATELSON ATTORNEY Nov. 23, 1965 s. NATELSON 3,219,416

APPARATUS FOR THE AUTOMATIC CHEMICAL SEQUENTIAL TREATMENT AND ANALYSIS OF SMALL QUANTITIES OF MATERIAL Filed Oct. 50, 1962 3 Sheets-Sheet 2 F 16. 1b it INVENTOR SAMUEL NATELSON Y BY fi ATTORNEY 3,219,416 EATMENT S. NATELSON Nov. 23, 1965 APPARATUS FOR THE AUTOMATIC CHEMICAL SEQUENTIAL TR AND ANALYSIS OF SMALL QUANTITIES OF MATERIAL Filed Oct. 30, 1962 3 Sheets-Sheet 5 6 NT a A mL U 5 M mm L Y B N: L m: IH@ w m f A:

ATTORNEY United States Patent 3,219,416 APPARATUS FOR THE AUTOMATIC CHEMICAL SEQUENTIAL TREATMENT AND ANALYSIS OF SMALL QUANTITIES 0F MATERIAL Samuel Natelson, Valley Stream, N.Y., assignor to Scientific Industries, Inc., Springfield, Mass, a corporation of Delaware Filed Oct. 30, 1962, Ser. No. 234,019 Claims. (Cl. 23-253) The present invention is a continuation-in-part of the Samuel Natelson, United States patent application, Serial No. 170,084, filed January 31, 1962, which in turn is a continuation-in-part of United States patent application, Serial No. 14,894, filed March 14, 1960, now United States Patent No. 3,036,893. The present invention relates to automatic chemical treatment and analysis, and more particularly to the sequential treatment and analysis of samples.

The chemical laboratory is often faced with the problem of the analysis of large numbers of samples. This is time consuming and tedious to the operator often resulting in error due to the large number of samples being assayed and the close attention one must pay to each step of the procedure. The fatigue which sets in often results in errors being introduced. In many cases, several operators are required to finish the work of the day.

To relieve this condition, instruments have been introduced which automatically sample the material to be analyzed, add reagents, and go through elaborate processes both as regards procedure and instrument to perform the analysis automatically. In general, the instruments presently in use have been designed to mechanically reproduce the work performed by the human operator. Therefore, from the standpoint of time saving, these devices take about as much time to perform their function as their human counterpart. These instruments require appreciable amounts of material for analysis and do not lend themselves readily to adaption for the analysis of micro samples of the order microliters.

Modern hospitals must treat materail in drop quantity, often contained in a capillary tube. Present instruments although suited for test tube quantity of material are not suited for the rapid sequential analysis of capillary tubes. Present instruments are not equipped to handle capillary tubes. Indeed, proper discharge of material from such tubes is difiicult. No two materials act exactly alike. Not only are the viscosity and specific gravity a factor, but also the surface tension and afiinity of the liquid for the tube must be considered.

Athough many attempts may have been made to provide a device for the automatic rapid sequential treatment of substances contained in a capillary tube, none, as far as I am aware, were entirely satisfactory from the technical, scientific, chemical, commercial or industrial viewpoint.

It is therefore an object of the present invention to provide a device which can be used for the treatment and analysis of micro quantities of substances permitting the rapid sequential processing of a plurality of samples contained in capillary tubes.

' Another object of the present invention is to provide means for sequentially dispensing uniform small quantities of substances.

Still another object of the present invention is to provide a device which can treat and analyze substances contained in capillary tubes at a rapid pace.

With the foregoing and other objects in view, the invention resides in the novel arrangement and combination of parts, in the details of construction, and in the process steps hereinafter described and claimed, it being understood that changes in the precise embodiment of the invention herein disclosed may be made within the scope of what is claimed without departing from the spirit of the invention.

The invention will appear more clearly from the following detailed description when taken in connection with the accompanying drawing, showing by way of example, preferred embodiments of the inventive idea.

FIGURE 1 is a longitudinal perspective view of one embodiment of the inventive concept;

FIGURES 1a and 1b are a front and side view of one of the components shown in FIGURE 1;

FIGURE 2 depicts an exploded view of readout means used in connection with the embodiment of FIGURE 1;

FIGURE 3 shows a longitudinal perspective view of another embodiment of the inventive concept; and,

FIGURE 4 graphically explains the mathematical and geometric factors concerning the movement of the capillary tube.

In the first embodiment the capillary tubes are contained in an apparatus 12 designed to supply sequential samples into sample receiving means, e.g., receiving cups 13. The sample in the receiving cup will then be treated at a plurality of stations and finally a determination is to be provided at a reading station 14 along the path of travel of the receiving cups 13.

The sample will initially be contained in a capillary tube 15 which preferably should also have a funnel 16. This funnel may be separate from the capillary tube. The capillary tube is slipped into the elastic plastic bottom opening of the funnel and thus held rigidly; otherwise the capillary tube may have a funnel sealed to it. The capillary tube may be of glass or plastic. To process the sample therein, apparatus 12 is a turntable arrangement with a dispensing disc 17 and a plurality of radial slots 18 designed to house a dispensing assembly 19.

Cooperating with dispensing disc 17 is a support disc 20 for supporting the receiving cup 13. This support disc 20 is axially aligned with dispensing disc 17, both discs being turned simultaneously but intermittently on a shaft 21 as hereinafter described.

Dispensing assembly 19 includes radial beds 22 in slots 18 and the inner portion of the bed defines a radial track 23, having a guide wheel 24 therein. Affixed to guide wheel 24 is a tube holder 25 having a straight base portion 26 pivoted to guide wheel 24 at one end of said base portion and having clamp means 27 towards the other end. Extending radially from the base is a triangular flange 28 with an apex 29 opposite base portion 26.

The dispensing assembly 19 is so constructed and designed that a capillary tube 15 is normally held horizontally by the clamp means 27 funnel inward, and, when the capillary is tilted outwardly from the horizontal to the vertical position, the tip of the capillary will remain substantially over the same spot so that the contents of the capillary are discharged at one spot and not all over the discharge zone. This is accomplished by means of lever assembly 31. This lever assembly 31 is illustrated at both the left and right side of FIGURE 1, showing the action of the lever assembly when the capillary tube is in the vertical position on the left and when the capillary tube is in the horizontal position on the right.

Looking first at the lever assembly on the right, and assuming that the apparatus is at rest, it is noted that there is an outer lever arm 32 whose outer end is pivoted to the outer end 33 of bed 22. The inner end of outer lever arm is both pivoted to the apex 29 of triangular flange 28 and joined to one end of central lever arm 34.

It is observed at this point that by pushing up on central lever arm 34, as shown on the righthandside of the drawing, the tube holder moves outwardly, apex 29 is moved up, shifting capillary tube 15 from the vertical to the horizontal position. i

It is evident therefore from a study of the right and left side of the drawing that the central lever arm must be moved up and down at predetermined stations so as to change the position of the capillary tube held by the tube holder, up and back from horizontal to vertical by either pulling down or lifting up apex 29. This is accomplished by means of inner lever arm 35 pivoted to the inner end of central lever arm 34 and at its center to vertical fulcrum bar 36 on support disc 20. At both ends of inner lever arm 35 are horizontal pins 37 and 38 so that by pushing up on inner horizontal pin 37 opposite lever arm 34, the action of inner lever arm 35 pulls central lever arm 34 down and by pushing up on horizontal pin 38 at the juncture of central lever arm 34 and inner lever arm 35, arm 34 is pushed up.

' To move the capillary tube from the horizontal to the vertical position and back, it is therefore necessary to push up on the proper horizontal pin 37 or 38.

Still assuming for the time being that the apparatus is stationary, the moving of horizontal pins 37 and 38 is accomplished by means of cam assemblies 39 and 40. These assemblies operate in precisely the same manner except that assembly 39 will move horizontal pin 37 up to bring the'capillary tube to the vertical position whereas assembly 40 will move horizontal pin 38 to return the capillary tube to the horizontal position.

Each cam assembly consists of a cam housing 41 designed to permit a piston rod 42 to reciprocate vertically therein. At the upper end of the piston rod are pin engaging means 43, better shown in FIGURES la and lb. The horizontal pin of the inner lever arm is caught up in a mouth 44 while the lever arm itself will be caught in a hollow section 45. Mouth 44 is preferably of triangular shape whereas hollow section 45 is rectangular in shape. A spring 46 tends to keep engaging means out of engagement with the horizontal pin. The piston rod is moved up and down intermittently by rotating a chain and sprocket arrangement. One end of the chain 47 is aflixed to the lower end of the piston rod, the other end of the chain is aflixed to a revolving spoke 48. A sprocket 49 is intermediate both ends of the chain, and above the level of the revolving spoke 48 and the lower end of the piston. As the spoke rotates counterclockwise in the left assembly and clockwise in the right assembly, the chain is tightened and loosened. When tightened, the piston is forced up and the engaging means lift the horizontal pin. When the chain is loosened, the piston springs down again. Spoke 48 is turned by timed motor means 50.

Up to now the action described has been with relation to a stationary device. But the present device is not a stationary device. Indeed, there are in practice 40 capillary tubes on the turntable which are processed in about 200 seconds or a little more than three minutes.

To visualize this operation, it is necessary to imagine that a technician is standing at a loading station 51 placing capillary tubes 15 radially into the clamp means 27 with the funnel inward. The capillary tube thus lies horizontally in the tube holder. vanced to a sample receiving station 52 where the sample is discharged into a receiving cup 13 held or support disc 20 tilting the capillary tube to the horizontal position. From the discharge station the receiving cup will be moved to a plurality of treating stations for the purposes hereinafter explained.

Each station is seperated from the other station a fixed arcuate distance and the dispensing, disc and support disc must be moved intermittently along this distance, the intermittent'stop" time being sufficient for the desired function to be performed at the slowest station. Both discs are axially mounted on shaft 21 which is intermittently This tube is now to be ad-' driven by a motor and gear arrangement. This includes a drive motor 53 and a gear train 54. Drive motor 53 works in cooperation with the action of spoke 48. Piston rods 42 must pass through the support disc to engage the resective pins. Apertures 55 are provided in the support disc for this purpose. But rod 42 cannot move unless the support disc is stationary. Therefore a trip switch 56 is provided. As the spoke 48 turns, the end not attached to the chain comes around and trips switch 56. This strats motor 53. A timer controls the motor and the rate of rotation of the spoke. A second trip switch 57 coupled to the gearing of motor 53 then takes over so as not to leave the turntable in an in-between position. This second trip switch assures that the turntable will turn one station.

Therefore, after the technician has inserted the capillary tube horizontally in the clamp at the station 51, the tube moves to sample receiving station 52. Here the turntable stops, horizontal pin 38 is engaged by the engaging means on the piston rod moving through aperture 55 and the tube is tilted to the vertical position to enter receiving cup 13. Piston rod 42 is lowered and the engaging means are below the support disc. The turntable moves over to the next' station which is wash station 58. Now the capillary tube is washed through with a solvent, from a spout 59 which is positioned above the station. Again, turntable moves over to the next station which is reagent station 60 having a bent tube 61 to supply reagent to the receiving cup, from a source (not shown). The turntable then moves again to a gas feed station 62. Here, air or an inert gas is forced through the capillary tube causing turbulence in the receiving cup to mix the materials therein and to complete the emptying of the capillary. Finally the turntable reaches vertical to horizontal tilting station 63 where the action has already been described. Here the engaging means on the piston rod will engage the horizontal pin at the junction of the inner and central lever arms. Past the vertical to horizontal station is reading station 14.

Reading station 14 includes a light source 64, under the support disc, a collimating lens 65 to make the rays parallel, a light filter 66 to produce a monochromatic light, a diaphragm 67 to narrow the beam so that it is no wider than the cup. The cup itself has a flanged bottom for stability. Over the cup is a photocell 68 attached to a readout device 69 such as a recorder or a digital readout so as to yield the result.

The embodiment just described has the capillary tubes tilting outwards. It is also possible to construct a device with the capillary tubes tilting inwards. Thus, in embodiment 112 of FIGURE 3, the capillary tube 15 tilts inward. This arrangement is shown in connection with the dispensing of the sample on a moving tape means 113. The treatment and analysis of such samples on tube means has already been described in the Samuel Natelson, US. Patent No. 3,036,893, and for the purpose of describing the present invention there is shown briefly a sample receiving tape, a pay-off reel 114 holding tape means 1'13, which moves on to a sample receiving station 115 over a guide roller 116 and from there to squeeze guide rollers 116, which are designed to intermittently move the tape. The intermittent motion is provided by motor means 117 and gearing 118.

The sample is placed on the tape using a dispensing disc 119 with a plurality of radial slots 120 housing a dispensing assembly 121 including a bed 122 radially disposed in slots 120. Since the capillary tube will be tilted inwardly this time, the outward portion of the bed defines a radial track 123 with a guide wheel 124 therein. Aflixed to guide wheel 124 isa tube holder 12-5 having the previously described straight base portion 126 pivoted to guide Wheel 124. At one end of this base portion are clamp means 127, and towards the other end, extending radially from the base is a triangular flange 128 with an apex 129 opposite base portion 126.

that is, cam end 134 is normally down.

This dispensing assembly is so constructed and designed that a capillary tube 15 is normally held horizontally by the clamp means 127, funnel outward, and when the capillary tube is tilted inward from the horizontal to the vertical position, the tip of the capillary tube will remain substantially over the same spot so that the contents of the capillary are discharged at one spot and not all over the discharge zone. In this embodiment, a lever 130 is pinned to the apex 129 of flange 128 and to the inward end of the straight base portion of the bed 122. The end of lever 130 terminates in bearing means 131 shown as a wheel pinned to the end of the lever. As can be seen from the drawing, the capillary tube is normally held in the horizontal position because of the action of a spring 133 in the flange 128. As the capillary tube reaches the sample receiving station 115, bearing means 131 are engaged by the cam end 134 of a "bent, two arm lever 135. Lever 135 is pivoted at the junction of its arms, to a stationary support 136. The action of lever 136 is such, However, the cam end is brought upwards as the capillary tubes sequentially reach the sample receiving station. To this end, the inner end of two arm lever 135 has second bearing means 137 in engagement with an eccentric wheel 138 driven by motor 139. Second bearing means 137 are kept in engagement with eccentric wheel 138 by a spring 140. Eccentric wheel 138 is constantly driven by a timing motor 141. When cam end 134 of lever '135 moves down, it presses down on contact 142 which starts drive motor 143 and tape motor 117. Drive motor 143 starts the gearing 144 which will turn the central shaft 145 to turn the disc. Coupled to drive motor 143 is a second contact 146 activated by the gearing. This second contact assures that the dispensing disc will turn one full station and not stop in between. Movement will not start again until the cam moves up again and then down, pressing again on switch 142. Thus each time switch 142 is pressed the turntable moves one station and stops.

From the foregoing description, it is apparent that in delivering a sample from capillaries it is advantageous that the tip of the capillary be at all times above the same spot when the capillary tilts. This is of special importance with wider capillaries where a drop will fall out when the capillary is tilted a particular angle. Finally when the capillary is in the vertical position and a second drop falls or is blown out of the capillary it must fall in the same place as the initial drop. Otherwise, one might lost part of the sample, or if transferred to paper, one will not obtain a circular spot.

This can be accomplished in two distinct motions. If the capillary is attached to a hinged support as described in my co-pending application #170,084, with the tip in juxtaposition to the pivot of the hinge and perpendicular to said pivot, the tip of the capillary will stay in the same position as the hinge is opened. If desired the capillary may then be moved down in a separate motion after the capillary is in the vertical position. A variation of this motion is to slide the hinge support backward while the hinge is being opened simultaneously.

A preferred system is to lift the capillary to its vertical position with the center of the capillary following a predetermined arc while the tip remains over the spot at all times. In this way the lifting of the capillary to the vertical and lowering of the capillary to the desired position can be accomplished in one smooth motion. The center of the capillary tube then describes an arc in its motion which is described by the equation.

When y and x are the rectilinear coordinates and a is half the length of the capillary tube.

C is the elevation of the capillary tube while in a horizontal position before tilting. log represents the logarithm to the base 10.

This equation derives from the geometry of FIGURE 4. In the figure, 1 is the capillary tube in the horizontal position before descending and is divided so that its length is 2:1, 2 or P representing the tube center which is to follow the are indicated by 3. 4 is the capillary tube now in any tilted position tangent to are 3 at its midpoint, P(x,y). The path to be described by the tip of the capillary 5 is the y axis. This tip will eventually move below the level of the x axis. The intercept of the tip of the capillary with the y axis is a distance b from the x axis.

A perpendicular from P(x,y) to the axis x (dotted line 6) will be a measure of y at any instant. A dotted line 7, drawn parallel to the x axis extending from the y axis to vertical line 6 is a measure of x at any instant during the lowering of the capillary. The length of the line extending from P(x,y) to line 7 can now be represented by (yb). Then by the law of right triangles we have Equation 2 Since the capillary tube is a straight line, we have the basic straight line equation.

Equation 4 (mx) -'|-x =zz Solving for the slope m we obtain 2 2 Equation 5 m= m Now the slope of the line and the curve at point P(x,y) at any instant in is equal to Thus we have Equation 6.

dy x a -:v Equation 6 x or for purposes of integration Integrating Equation 6 to obtain the value of y we obtain Equation 7.

dy dx Where C is the constant of integration and In represents the natural logarithm to the base 2. By multiplying by 2.3 we convert this to ordinary logarithms to the base 10 which is now in the form of Equation 1.

To evaluate the constant C we allow xin Equation 1 to be equal to a. y is then equal to C. Since x is equal to a only at the start when the capillary is in the horizontal position and y represents the height of the center of the capillary above the base level, therefore C then represents the height of the capillary tube from the horizontal axis before tilting.

It can be seen from Equation 1 that the capillary tube will be in the vertical position when x is equal to zero. This can theoretically never be reached with this motion constant number to the first term. Thus the motion in the capillary tilting device is a simultaneous double motion which simulates vthis equation to produce a smooth tilting and lowering of the capillary to keep the tip at all times above a fixed point so that a single spot is produced.

In the plot of FIGURE 4, the following values were used:

If C: 10 cm. and 11:4 cm., then These values assume that the capillary tube sets cm. above the table and the capillary tube is 8 cm. long. Of course, varying these two parameters will give different curves but not change the general slope of the curve. Varying C will only drop the curve if it is less and raise it if it is more than 10 cm. as used in the table. A C value of 10 cm. will keep the curve mainly in the upper right quadrant. Correspondence of the capillary tube with the y axis is only achieved as a limit.

It is to be observed therefore that the present invention provides for the sequential treatment and analysis of samples, and comprises in combination, dispensing means, e.g., a dispensing disc 17, 119, a plurality of capillary tube dispensing assemblies 19, 121, radially disposed on said dispensing means or disc, each assembly including means to hold a capillary tube therein; lever means 31, 131 coupled to each dispensing assembly to tilt the capillary tube held by the dispensing assembly so that the tip of the tube constantly remains over the same spot during tilting; a sample receiving station 52, 115 including tilting means 39, 135 designed to engage the lever means passing said station on the apparatus; and, intermittent moving means 53, 54, 143, 144 to intermittently move or rotate said dispensing means or disc in timed relation with the tilting of the capillary tube so as to bring each lever means to the sample receiving station. In the preferred embodiment, the tilting means 39 comprises a pair of cam assemblies each having a reciprocating rod 42, moving means 47, 48, 49, 50 to move the rod, and engaging means 43 to engage the lever means, one piston assembly so engaging the lever means as to tilt the capillary from the horizontal to the vertical position, the other piston assembly so engaging the lever assembly as to return the capillary tube from the vertical to the horizontal position. The dispensing disc 17 has a plurality of radial beds 22 housed in radial slots 18, each bed being designed to hold a dispensing assembly. The sample in the capillary is discharged into receiving cups 13 held on a support disc axially aligned, concentric with, and moving with the dispensing disc.

It .will be apparent to those skilled .in the art, that my present invention is not limited to the specific details described above and shown in the drawing, and that various modifications are possible in carrying out the features of the invention and the operation and method of support, mounting and utilization thereof, without departing from the spirit and scope of the appended claims.

I claim: 1

1.- An apparatus for the sequential treatment and analysis of samples contained in straight capillary tubes, comprising in combination;

circular dispensing means;

a plurality of capillary tube dispensing assemblies, radially disposed on said circular dispensing means, each assembly including means to hold a straight capillary tube therein;

lever means coupled to each dispensing assembly to tilt the straight capillary'tube held by the dispensing assembly so that the tip of the tube constantly remains over the same spot during tilting;

a station on the apparatus including tilting means designed to engage the lever means; and,

intermittent rotating means to intermittently rotate said circular dispensing means in timed relation with the tilting of the straight capillary tube.

2. An apparatus for the sequential treatment and analysis of samples contained in straight capillary tubes, comprising in combination;

circular dispensing means including a, dispensing disc for placing straight capillary tubes thereon and a support disc for placing sample receiving means thereon, said support disc being axially aligned and designed to rotate simultaneously with said dispensing disc;

a plurality of capillary tube dispensing assemblies, each assembly including means to hold a straight capillary tube therein;

lever means coupled to each dispensing assembly to tilt the straight capillary tube held by the dispensing assembly and discharge the contents thereof into the sample receiving means so that the tip of the tube constantly remains over the same spot during tilting;

a station on the apparatus including tilting means designed to engage the lever means associated with the apparatus;

intermittent rotating means to intermittently rotate said disc in timed'relation with the tilting of the straight capillary tube.

3. An apparatus as in claim 1 provided with means for adding reagents to develop a color so as to be evaluated at a reading station, and, a reading station comprising a light source projected vertically upward through the solution to a light detector coupled to readout means.

' 4. An apparatus for the sequential treatment and analysis of samples contained in capillaries, comprising in combination;

circular dispensing means including a dispensing disc for placing, capillary tubes thereon and a support disc for placing sample receiving means thereon, said support disc being axially aligned with and designed to rotate simultaneously with said dispensing disc;

a plurality of capillary tube dispensing assemblies, each assembly including a radial bed having a track and guide Wheel therein; a tube holder having a straight base portion pivoted to said guide wheel at one end having clamp means at the other end and a triangular flange whose apex is opposite said base portion;

lever means coupled to each dispensing assembly tube holder to tilt the capillary tube held by the tube holder so that the tip of the tube constantly remains directly over the same spot during tilting as the straight base portion one end pivoted to said guide wheel moves along said track;

a station on the apparatus including tilting means designed to engage the lever means associated with the apparatus;

intermittent rotating means to intermittently rotate said disc in timed relatiOn with the tilting of the capillary tube.

5. An apparatus for the sequential treatment and analysis of samples contained in capillaries, comprising in combination;

circular dispensing means including a dispensing disc for placing capillary tubes thereon and a support disc for placing sample receiving means thereon, said support disc being axially aligned with and designed to rotate with said dispensing disc;

a plurality of capillary tube dispensing assemblies radially disposed on said circular dispensing means, each assembly including means to hold a capillary tube therein;

lever means coupled to each dispensing assembly to tilt the capillary tube held by the dispensing assembly so that the tip of the tube constantly remains directly over the same spot during tilting;

two stations on the apparatus where said capillary tube is tilted from the horizontal to the vertical and from the vertical to the horizontal including, piston assemblies at each station, each assembly having a reciprocating rod, moving means to intermittently move the rod, and engaging means to engage the lever means, one piston assembly so engaging the lever means as to tilt the capillary tube from the horizontal to the vertical position, the second piston assembly so engaging the lever means as to return the capillary tube from the vertical to the horizontal position; and,

intermittent rotating means to intermittently rotate said disc in timed relation with the reciprocations of said rods.

6. An apparatus for the sequential treatment and analysis of samples contained in capillaries, comprising in combination;

circular dispensing means including a dispensing disc for placing capillary tubes thereon and a support disc for placing sample receiving means thereon, said support disc being axially aligned with and designed to rotate with said dispensing disc;

a plurality of capillary tube dispensing assemblies, each assembly including a radial bed having a track and guide wheel therein, a tube holder having a straight base portion pivoted to said guide Wheel at one end and having clamp means at the other end and a triangular flange whose apex is opposite said base portion;

lever means coupled to each dispensing assembly to outwardily tilt the capillary tube held by the dispensing assembly so that the tip of the tube constantly remains over the same spot during tilting, said lever means including an outer lever arm whose outer end is pivoted to the outer end of the radial bed, the inner end being pivoted to said apex and joined to one end of a central lever arm, an inner arm and a fulcrum bar, said other end of said central lever arm being pivoted to said inner lever arm one end, said inner lever arm being pivoted to said fulcrum bar at its center and, having horizontal pins at the inner and outer ends of said inner lever arm;

two stations on the apparatus for tilting said capillary tube from the horizontal to the vertical and from the vertical to the horizontal, including tilting means at each station designed to engage the one or the other of said pins, pushing up on the pin to tilt the capillary tube, the one tilting means engaging the pin at the inner end, the other tilting means engaging the pin at the outer end of said inner lever arm; and,

intermittent rotating means to intermittently rotate said disc in timed relation with the tilting of the capillary tube.

7. An apparatus as claimed in claim 6, said tilting means including piston assemblies at each station, each assembly having a reciprocating rod, moving means to intermittently move the rod, and engaging means to engage the lever means.

8. An apparatus as claimed in claim 7, said moving means to intermittently move the rod including a chain and sprocket arrangement, having a chain, one end of said chain being aflixed to the lower end of said rod, a revolving spoke, the other end of said chain being aflixed to one end of said spoke, and a sprocket intermediate said spoke and rod lower end and above the horizontal level thereof, and timed motor means to turn said spoke.

9. An apparatus as claimed in claim 8, said intermittent rotating means to intermittently rotate said discs in timed relation with the tilting of the capillary tube including a shaft on which said discs are mounted, a drive motor and gear arrangement for driving said shaft, and a trip switch means at one of said stations connected to said drive motor, said trip switch being closed by the other end of said revolving spoke as it turns around.

10. An apparatus as claimed in claim 9 including a second trip switch coupled to said gear arrangement which takes over once said motor starts assuring that said shaft will turn said discs a predetermined distance.

References Cited by the Examiner UNITED STATES PATENTS 1,097,708 5/ 1914 Elson 23-259 1,643,243 9/ 1927 Hatfield.

2,113,063 4/1938 Stryken et a1 23230 X 2,867,355 1/1959 Jones 222-194 X MORRIS O. WOLK, Primary Examiner.

JAMES H. TAYMAN, JR., Examiner.

Claims (1)

1. AN APPARATUS FOR THE SEQUENTIAL TREATMENT AND ANALYSIS OF SAMPLES CONTAINED IN STRAIGHT CAPILLARY TUBES, COMPRISING IN COMBINATION; CIRCULAR DISPENSING MEANS; A PLURALITY OF CAPILLARY TUBE DISPENSING ASSEMBLIES, RADIALLY DISPOSED ON SAID CIRCULAR DISPENSING MEANS, EACH ASSEMBLY INCLUDING MEANS TO HOLD A STRAIGHT CAPILLARY TUBE THEREIN; LEVER MEANS COUPLED TO EACH DISPENSING ASSEMBLY TO TILT THE STRAIGHT CAPILLARY TUBE HELD BY THE DISPENSING ASSEMBLY SO THAT THE TIP OF THE TUBE CONSTANTLY REMAINS OVER THE SAME SPOT DURING TILTING; A STATION ON THE APPARATUS INCLUDING TILTING MEANS DESIGNED TO ENGAGE THE LEVER MEANS; AND, INTERMITTENT ROTATING MEANS TO INTERMITTENTLY ROTATE SAID CIRCULAR DISPENSING MEANS IN TIMED RELATION WITH THE TILTING OF THE STRAIGHT CAPILLARY TUBE.
US3219416A 1962-10-30 1962-10-30 Apparatus for the automatic chemical sequential treatment and analysis of small quantities of material Expired - Lifetime US3219416A (en)

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US3219416A US3219416A (en) 1962-10-30 1962-10-30 Apparatus for the automatic chemical sequential treatment and analysis of small quantities of material

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Cited By (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3302452A (en) * 1964-04-27 1967-02-07 Cutler Hammer Inc Coagulation detector and coagulability determination
US3432271A (en) * 1966-05-02 1969-03-11 American Instr Co Inc Automatic analytical apparatus
US3489521A (en) * 1965-04-14 1970-01-13 Vickers Ltd Automatic laboratory
US3525592A (en) * 1966-09-13 1970-08-25 Quickfit & Quartz Ltd Sampling and diluting apparatus
US3547781A (en) * 1968-01-22 1970-12-15 Automatisme Cie Gle Filling line for the filling of containers
US3615236A (en) * 1968-03-19 1971-10-26 Bodenseewerk Perkin Elmer Co Apparatus for automatic chemical analyses
JPS50104981A (en) * 1974-01-25 1975-08-19
JPS51108887A (en) * 1975-03-20 1976-09-27 Nippon Electron Optics Lab Jidokagakubunsekisochi
JPS51108888A (en) * 1975-03-20 1976-09-27 Nippon Electron Optics Lab Jidokagakubunsekisochitoyokaitenhannoki
US4067694A (en) * 1976-12-17 1978-01-10 Eastman Kodak Company Loading and unloading mechanism for continuously rotating container
US4186187A (en) * 1972-07-24 1980-01-29 California Institute Of Technology Sample processor for the automatic extraction of families of compounds from liquid samples and/or homogenized solid samples suspended in a liquid
USRE30562E (en) * 1979-02-22 1981-03-31 Immunological testing devices
US4340390A (en) * 1980-06-16 1982-07-20 Eastman Kodak Company Method and apparatus for metering biological fluids
EP0083474A1 (en) * 1981-12-01 1983-07-13 The Upjohn Company Microprocessor controllable automatic sampler
US4508148A (en) * 1983-05-06 1985-04-02 Tl Systems Corporation Pharmaceutical filler apparatus
US4855110A (en) * 1987-05-06 1989-08-08 Abbott Laboratories Sample ring for clinical analyzer network
US4912986A (en) * 1987-04-03 1990-04-03 Avl Ag Device for the selective charging of an analysing apparatus
US5002103A (en) * 1988-09-22 1991-03-26 Nuova Zanasi S.P.A. Apparatus for adjusting the volume of dippable hollow punch dosing devices
US5311913A (en) * 1992-02-08 1994-05-17 Eastman Kodak Company Dispersion preparation method
US5339875A (en) * 1992-02-08 1994-08-23 Eastman Kodak Company Liquid preparation method
US5585068A (en) * 1990-02-20 1996-12-17 Biochemical Diagnostics, Inc. Apparatus for automatically separating a compound from a plurality of discrete liquid specimens
WO1997046712A2 (en) * 1996-06-04 1997-12-11 University Of Utah Research Foundation System and method for carrying out and monitoring biological processes
US5935522A (en) * 1990-06-04 1999-08-10 University Of Utah Research Foundation On-line DNA analysis system with rapid thermal cycling
US6174670B1 (en) 1996-06-04 2001-01-16 University Of Utah Research Foundation Monitoring amplification of DNA during PCR
US20020044894A1 (en) * 1999-12-13 2002-04-18 Michal Lebl Oligonucleotide synthesizer
US6827901B2 (en) 1990-03-02 2004-12-07 Ventana Medical Systems, Inc. Automated biological reaction apparatus
US20050064582A1 (en) * 1990-06-04 2005-03-24 University Of Utah Research Foundation Container for carrying out and monitoring biological processes
US20060085140A1 (en) * 2002-12-20 2006-04-20 Gordon Feingold Information notification sample processing system and methods of biological slide processing
US7081226B1 (en) 1996-06-04 2006-07-25 University Of Utah Research Foundation System and method for fluorescence monitoring
US7270785B1 (en) 2001-11-02 2007-09-18 Ventana Medical Systems, Inc. Automated molecular pathology apparatus having fixed slide platforms
US7303725B2 (en) 2002-04-15 2007-12-04 Ventana Medical Systems, Inc. Automated high volume slide staining system
US7378055B2 (en) 2002-04-26 2008-05-27 Ventana Medical Systems, Inc. Automated molecular pathology apparatus having fixed slide platforms
US7468161B2 (en) 2002-04-15 2008-12-23 Ventana Medical Systems, Inc. Automated high volume slide processing system
US20100154207A1 (en) * 2008-12-23 2010-06-24 Optimize Technologies, Inc. Assembly for placing an insert into communication with an analytical chemical instrument
WO2010078177A1 (en) * 2008-12-31 2010-07-08 Ventana Medical Systems, Inc. Robotic pipette system

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US1097708A (en) * 1913-11-18 1914-05-26 Harry E Elson Machine for washing precipitates.
US2113063A (en) * 1935-04-08 1938-04-05 Albert R Stryker Fluid testing apparatus
US2867355A (en) * 1954-09-02 1959-01-06 Jones Alan Richardson Apparatus and methods useful in the preparation of precise dilutions of liquids

Cited By (84)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3302452A (en) * 1964-04-27 1967-02-07 Cutler Hammer Inc Coagulation detector and coagulability determination
US3489521A (en) * 1965-04-14 1970-01-13 Vickers Ltd Automatic laboratory
US3432271A (en) * 1966-05-02 1969-03-11 American Instr Co Inc Automatic analytical apparatus
US3525592A (en) * 1966-09-13 1970-08-25 Quickfit & Quartz Ltd Sampling and diluting apparatus
US3547781A (en) * 1968-01-22 1970-12-15 Automatisme Cie Gle Filling line for the filling of containers
US3615236A (en) * 1968-03-19 1971-10-26 Bodenseewerk Perkin Elmer Co Apparatus for automatic chemical analyses
US4186187A (en) * 1972-07-24 1980-01-29 California Institute Of Technology Sample processor for the automatic extraction of families of compounds from liquid samples and/or homogenized solid samples suspended in a liquid
JPS546236B2 (en) * 1974-01-25 1979-03-26
JPS50104981A (en) * 1974-01-25 1975-08-19
JPS51108887A (en) * 1975-03-20 1976-09-27 Nippon Electron Optics Lab Jidokagakubunsekisochi
JPS51108888A (en) * 1975-03-20 1976-09-27 Nippon Electron Optics Lab Jidokagakubunsekisochitoyokaitenhannoki
JPS5340915B2 (en) * 1975-03-20 1978-10-30
JPS5334079B2 (en) * 1975-03-20 1978-09-19
US4067694A (en) * 1976-12-17 1978-01-10 Eastman Kodak Company Loading and unloading mechanism for continuously rotating container
USRE30562E (en) * 1979-02-22 1981-03-31 Immunological testing devices
US4340390A (en) * 1980-06-16 1982-07-20 Eastman Kodak Company Method and apparatus for metering biological fluids
EP0083474A1 (en) * 1981-12-01 1983-07-13 The Upjohn Company Microprocessor controllable automatic sampler
US4508148A (en) * 1983-05-06 1985-04-02 Tl Systems Corporation Pharmaceutical filler apparatus
US4912986A (en) * 1987-04-03 1990-04-03 Avl Ag Device for the selective charging of an analysing apparatus
US4855110A (en) * 1987-05-06 1989-08-08 Abbott Laboratories Sample ring for clinical analyzer network
US5002103A (en) * 1988-09-22 1991-03-26 Nuova Zanasi S.P.A. Apparatus for adjusting the volume of dippable hollow punch dosing devices
US5585068A (en) * 1990-02-20 1996-12-17 Biochemical Diagnostics, Inc. Apparatus for automatically separating a compound from a plurality of discrete liquid specimens
US7470541B2 (en) 1990-03-02 2008-12-30 Ventana Medical System, Inc. Automated biological reaction apparatus
US6827901B2 (en) 1990-03-02 2004-12-07 Ventana Medical Systems, Inc. Automated biological reaction apparatus
US6943029B2 (en) 1990-03-02 2005-09-13 Ventana Medical Systems, Inc. Automated biological reaction apparatus
US7273749B1 (en) 1990-06-04 2007-09-25 University Of Utah Research Foundation Container for carrying out and monitoring biological processes
US7745205B2 (en) * 1990-06-04 2010-06-29 University Of Utah Research Foundation Container for carrying out and monitoring biological processes
US20050064582A1 (en) * 1990-06-04 2005-03-24 University Of Utah Research Foundation Container for carrying out and monitoring biological processes
US5935522A (en) * 1990-06-04 1999-08-10 University Of Utah Research Foundation On-line DNA analysis system with rapid thermal cycling
US5311913A (en) * 1992-02-08 1994-05-17 Eastman Kodak Company Dispersion preparation method
US5339875A (en) * 1992-02-08 1994-08-23 Eastman Kodak Company Liquid preparation method
EP1442794A2 (en) * 1996-06-04 2004-08-04 University Of Utah Research Foundation System and method for carrying out and monitoring biological processes
US6245514B1 (en) 1996-06-04 2001-06-12 University Of Utah Research Foundation Fluorescent donor-acceptor pair with low spectral overlap
US6569627B2 (en) 1996-06-04 2003-05-27 University Of Utah Research Foundation Monitoring hybridization during PCR using SYBR™ Green I
US6232079B1 (en) 1996-06-04 2001-05-15 University Of Utah Research Foundation PCR method for nucleic acid quantification utilizing second or third order rate constants
US6174670B1 (en) 1996-06-04 2001-01-16 University Of Utah Research Foundation Monitoring amplification of DNA during PCR
EP1493826A1 (en) * 1996-06-04 2005-01-05 University Of Utah Research Foundation Container for carrying out and monitoring biological processes
WO1997046707A3 (en) * 1996-06-04 1998-10-08 David R Hillyard System and method for monitoring for dna amplification by fluorescence
EP1442794A3 (en) * 1996-06-04 2005-05-11 University Of Utah Research Foundation System and method for carrying out and monitoring biological processes
WO1997046712A3 (en) * 1996-06-04 1998-05-07 David R Hillyard System and method for carrying out and monitoring biological processes
US20060029965A1 (en) * 1996-06-04 2006-02-09 Wittwer Carl T System for fluorescence monitoring
WO1997046707A2 (en) * 1996-06-04 1997-12-11 University Of Utah Research Foundation System and method for monitoring for dna amplification by fluorescence
US20090258414A1 (en) * 1996-06-04 2009-10-15 Wittwer Carl T System for fluorescence monitoring
US7081226B1 (en) 1996-06-04 2006-07-25 University Of Utah Research Foundation System and method for fluorescence monitoring
US7670832B2 (en) 1996-06-04 2010-03-02 University Of Utah Research Foundation System for fluorescence monitoring
WO1997046712A2 (en) * 1996-06-04 1997-12-11 University Of Utah Research Foundation System and method for carrying out and monitoring biological processes
US20090311673A1 (en) * 1996-06-04 2009-12-17 Wittwer Carl T Nucleic acid amplification methods
EP1674585A1 (en) * 1996-06-04 2006-06-28 University Of Utah Research Foundation Apparatus for performing PCR and monitoring the reaction in real time during temperature cycling
US8465694B2 (en) 1999-12-13 2013-06-18 Illumina, Inc. Oligonucleotide synthesizer
US7390459B2 (en) * 1999-12-13 2008-06-24 Illumina, Inc. Oligonucleotide synthesizer
US20020044894A1 (en) * 1999-12-13 2002-04-18 Michal Lebl Oligonucleotide synthesizer
US20090023605A1 (en) * 1999-12-13 2009-01-22 Michal Lebl Oligonucleotide synthesizer
US20110143965A1 (en) * 1999-12-13 2011-06-16 Michal Lebl Oligonucleotide synthesizer
US7404927B2 (en) 2001-11-02 2008-07-29 Ventana Medical Systems, Inc. Automated molecular pathology apparatus having fixed slide platforms
US7270785B1 (en) 2001-11-02 2007-09-18 Ventana Medical Systems, Inc. Automated molecular pathology apparatus having fixed slide platforms
US9528918B2 (en) 2002-04-15 2016-12-27 Ventana Medical Systems, Inc. Automated high volume slide processing system
US7303725B2 (en) 2002-04-15 2007-12-04 Ventana Medical Systems, Inc. Automated high volume slide staining system
US7468161B2 (en) 2002-04-15 2008-12-23 Ventana Medical Systems, Inc. Automated high volume slide processing system
US8663991B2 (en) 2002-04-15 2014-03-04 Ventana Medical Systems, Inc. Automated high volume slide processing system
US8048373B2 (en) 2002-04-15 2011-11-01 Ventana Medical Systems, Inc. Automated high volume slide staining system
US7378055B2 (en) 2002-04-26 2008-05-27 Ventana Medical Systems, Inc. Automated molecular pathology apparatus having fixed slide platforms
US8216512B2 (en) 2002-12-20 2012-07-10 Dako Denmark A/S Apparatus for automated processing biological samples
US7937228B2 (en) 2002-12-20 2011-05-03 Dako Denmark A/S Information notification sample processing system and methods of biological slide processing
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US7758809B2 (en) 2002-12-20 2010-07-20 Dako Cytomation Denmark A/S Method and system for pretreatment of tissue slides
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US8257968B2 (en) 2002-12-20 2012-09-04 Dako Denmark A/S Method and apparatus for automatic staining of tissue samples
US8298815B2 (en) 2002-12-20 2012-10-30 Dako Denmark A/S Systems and methods of sample processing and temperature control
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US8386195B2 (en) 2002-12-20 2013-02-26 Dako Denmark A/S Information notification sample processing system and methods of biological slide processing
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US7648678B2 (en) 2002-12-20 2010-01-19 Dako Denmark A/S Method and system for pretreatment of tissue slides
US8529836B2 (en) 2002-12-20 2013-09-10 Dako Denmark A/S Apparatus for automated processing biological samples
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US8788217B2 (en) 2002-12-20 2014-07-22 Dako Denmark A/S Information notification sample processing system and methods of biological slide processing
US8969086B2 (en) 2002-12-20 2015-03-03 Dako Denmark A/S Enhanced scheduling sample processing system and methods of biological slide processing
US9778273B2 (en) 2002-12-20 2017-10-03 Dako Denmark A/S Isolated communication sample processing system and methods of biological slide processing
US8307541B2 (en) 2008-12-23 2012-11-13 Optimize Technologies, Inc. Assembly for placing an insert into communication with an analytical chemical instrument
US20100154207A1 (en) * 2008-12-23 2010-06-24 Optimize Technologies, Inc. Assembly for placing an insert into communication with an analytical chemical instrument
WO2010078177A1 (en) * 2008-12-31 2010-07-08 Ventana Medical Systems, Inc. Robotic pipette system

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