US3929411A - Sample transfer device and method for analytical system - Google Patents
Sample transfer device and method for analytical system Download PDFInfo
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- US3929411A US3929411A US39229473A US3929411A US 3929411 A US3929411 A US 3929411A US 39229473 A US39229473 A US 39229473A US 3929411 A US3929411 A US 3929411A
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1095—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers
- G01N35/1097—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers characterised by the valves
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00465—Separating and mixing arrangements
- G01N2035/00534—Mixing by a special element, e.g. stirrer
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
- G01N2035/1025—Fluid level sensing
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/8593—Systems
- Y10T137/86187—Plural tanks or compartments connected for serial flow
- Y10T137/86196—Separable with valved-connecting passage
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/11—Automated chemical analysis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
- Y10T436/2575—Volumetric liquid transfer
Definitions
- An apparatus for chemical treatments has an enclosed vessel provided withlines for conveying samples and selectively openable valves in communication with sources of gases at atmospheric, increased, and reduced pressures.
- a plurality of such vessels may be combined, instead, in which case the pressure of the atmosphere in each vessel is made higher than that in the following vessel, so that the sample can be transferred to the following vessels.
- the vessel or vessels may be equipped with means for agitation, fixedquantity sampling, liquid level detection, washing, filtration, extraction, thermostatic control, aeration, thermal concentration and distillation.
- An additional vessel equipped with pH-adjusting means and capable of maintaining an atmospheric pressure inside may be installed.
- FIG. 2 PRIOR ART
- FIG. 3 PRIOR ART U.S. Patent Dec. 30, 1975 Sheet 2 of 12 3,929,411
- FIG. 4 PRIOR ART +-T k 26a 27 26b 27 26c US. Patent Dec. 30, 1975 Sheet 3 of 12 3,929,411
- FIG.5 PRIOR ART US. Patent Dec. 30, 1975 Sheet4 of 12 3,929,411
- each sample to be handled ranges in volume from ml to 200 ml (or even 500 ml in some cases). From the viewpoint of the conveyance of samples in such volumes, the conventional methods have not proved satisfactory for the reasons to be explained later. Establishment of a new conveyance system has, therefore, been urgently needed for the perfection of automatic chemical analyses.
- One of the method uses a continuous flow divided by air bubbles into small-quantity portions. Wherein a reagent line merges with a main sample line and an air line is open into the sample line downstream of said merging point of the reagent line. All these lines are made of elastic material and the sample line and associated lines are squeezed by a squeeze pump having rollers to convey the contents forward, thereby air bubbles equidistantly join the flow of sample-reagent mixture to divide the same into equal portions. Thenceforth the sample-reagent mixture and air bubbles alternately form a stream and move altogether through the main sample line.
- This method has the following limitations.
- the sample pipe to be used must have an inner diameter small enough to avoid the disappearance of air bubbles therein, and this places an important limitation upon the quantity of the sample that can be handled.
- the arrangement is not adapted for such chemical treatment as extraction and dissolution of solids.
- the inside diameters of the lines which may be chosen are actually limited and only a few sizes are available. This confines the mixing ratio of the reagent and sample within a certain range.
- the pipes to be used must be elastic enough to endure squeezing and must be chemically stable to the sample and reagent to be encoun- 2 tered. Because of these limitations, some special method must be developed and adopted.
- Another known method consists of retaining a sample in a container chemically treating the sample, and then transferring the sample to another place where it is to be subjected to another chemical treatment, either by moving the vessel or drawing up the sample by suction into the pipetter and discharging the same into another vessel.
- This method also has some limitations. It is impossible in this method to perform such chemical operations as extractive filtration, and distillation.
- the volume that the pipetter can handle is limited.
- the fact that the reaction vessels have to be moved together makes it necessary to handle only a small quantity of sample or even to adopt a special analytical procedure.
- the moving part of the equipment tend to be complicated in structure and increased in size. The sample is exposed to the atmosphere.
- a third method known in the art is to convey a sample gravitationally by natural dropping.
- This method is characterized by the retention of the sample in a vessel during its chemical treatment and by the dependence upon natural downflow by gravity for the transport of the sample and the like.
- the transfer lines must be held as vertically as possible and therefore the components parts that may be used are limited.
- a variety of samples cannot be smoothly handled.
- Each border of each reaction tank or the like requires a valve. To reduce the resistance of the pipes and valves is of value in facilitating the transport of the sample but brings a penalty of increased dead space, which in turn may cause undesirable intermingling of different samples when they are to be analyzed in succession.
- the present invention has been perfected with the view to eliminating the foregoing disadvantages of the prior art equipment, and has for an object to provide a large-capacity apparatus for chemical treatments adapted for practicing a novel method of transporting fluids and capable of chemically analyzing many different samples.
- Another object of the invention is to provide an apparatus for chemical treatments capable of automatizing all of the chemical analytical procedures that can be manually performed.
- Still another object of the invention is to provide an apparatus for chemical treatments which can be increased in capacity and easily adapted for modifications in analytical procedures.
- a further object of the invention is to provide an apparatus for chemical treatments capable of handling solid samples as well as fluid ones, with the system hermetically sealed.
- an apparatus for chemical treatments which comprises closed vessels, groups of lines and selectively openable valves provided on the upper and bottom parts of the vessels for the conveyance of sample, an atmospheric-pressure gas source, an increased-pressure gas source, and a reduced-pressure gas source, said sources being communicated with said valve groups, one for each, said valve groups being selectively operated to control the pressure of the atmosphere in said vessels so that the sample can be transferred from the outside into the vessels or vice versa.
- FIGS. 1 and 2 are diagrammatic views illustrating the conveyance of sample by a prior art technique
- FIGS. 3 and 4 are schematic sectional views of an automatic analyzer of a known type
- FIG. 5 is a schematic sectional view of an automatic analyzer of another known type
- FIg. 6 is a schematic view explanatory of the principle of fluid conveyance for the chemical apparatus according to this invention.
- FIG. 7 is a schematic view illustrating connections for the apparatus of the invention.
- FIG. 8 is a schematic view of a unit equipment of the apparatus according to the invention.
- FIGS. 9 through 21 are schematic views of other unit equipments according to the invention.
- FIG. 22 is a schematic view of an arrangement for chemical treatments embodying the invention.
- FIGS. 23 and 24a are diagrammatic sectional view of other forms of unit equipments embodying the invention and FIG. 24b is a sectional view along the line XXIVb-XXIVb of FIG. 24a.
- FIGS. 1 to 5 Before explaining the present invention with reference to embodiments thereof shown in the drawings, the three methods employed in the existing automatic analyzers will now be described more definitely by referring to FIGS. 1 to 5.
- FIGS. 1 and 2 schematically show the concept of the first prior method using a continuous flow divided by air bubbles into small-quantity portions.
- a reagent line 7 merges with a main sample line 6 at a junction 9, whereas an air line 4 is open into the sample line at a junction 10.
- a plurality of rollers 11, 11', are connected with chains 12 to constitute a squeeze pump, generally indicated at 13, which is driven in the direction indicated by an arrow in FIG. 2, so that the sample line 1 and the associated lines can be squeezed to convey the contents forward.
- the quantities of the sample and other fluids that flow through them depend primarily upon the inner cross sectional areas of the respective lines.
- a sample 1 runs in the sample line 6, a reagent 2 in the reagent line 7, and clean air 4 in the air line 8.
- the reagent 2 first merges into the sample 1 at the junction 9 to form a sample-reagent mixture 3, and then air bubbles 5 enter the mixture at the junction 10.
- the mixing ratio of the sample 1 to the reagent 2 is governed by the ratio of the inner cross sectional area of the sample line 6 to that of the reagent line 7.
- the air bubbles 5 equidistantly join the flow of the sample-reagent mixture 3 at the intervals dictated by the ratio of the inner cross sectional area of the air line 8 to the sum of the inner cross sectional areas of the sample line 6 and reagent line 7, thereby dividing the sample-reagent mixture 3 into equal portions.
- Each of the air bubbles 5 serves as a barrier wall to avoid intermixing of the adjacent sample-reagent mixture portions. Thenceforth the sample-reagent mixture 3 and air bubbles 5 alternately form a stream and move altogether through the main sample line 6.
- a reagent can be added at a suitably controlled rate to a continuous flow of sample, and a desirable period of time for a chemical reaction can be obtained through a judicious choice of line length.
- the sample pipe to be used must have an inner diameter small enough to avoid the disappearance of air bubbles therein. Practically the upper limit of the diameter is about 5 mm, and this places an important limitation upon the capacity of the sample line, or the flow rate of the sample that can be handled. In addition, the arrangement is not adapted for such chemical treatments as extraction and dissolution of solids.
- the inside diameters of the lines which may be chosen are actually limited and only a few sizes are available. Consequently the mixing ratio of the reagent and sample is confined within a certain range.
- the pipes to be employed must be elastic enough to endure squeezing and must be chemically inert to the sample and reagent to be encountered. Because of these requirements, some special method must be developed and adopted. Thus, as compared to other approaches, the method has major limitiations in limitations chemical analyses involved and in the accuracy or reliability of the results.
- FIGS. 3 and 4 schematically represent the concept of the second known method consisting the steps of retaining a sample in a container, chemically treating the sample, and then transferring the sample to another place where it is to be subjected to another chemical treatment, either by moving the vessel or drawing up the sample by suction and discharging the same into another vessel.
- reaction vessels 26a, 26b, 260 are connected with chains 27 in an orderly manner and are moved stepwise by drives (not shown) in the direction indicated by an arrow.
- a pipetter, designated 28, is capable of drawing up by suction the contents of a reaction vessel or discharging the contents into an empty vessel through a nozzle 29 equipped with drives (not shown) for its vertical and horizontal movements.
- a dispenser 24 is operatively connected to two valves 25, so that a reagent 22 from a reagent bottle 33 can be admitted into a reaction vessel via lines 31, 32 and through a nozzle 30 equipped with drives (not shown) for its vertical movement.
- the nozzle 30 may be independent of the nozzle 29 or may be connected thereto with a bridging tube 34.
- the sample can be transferred from one place to another where another chemical operation is to be performed, in either of two ways.
- One way is to cause the pipetter 28 to draw up by suction the contents of a reaction vessel (e.g., the vessel 26b) by way of the nozzle 29,
- the nozzle 29 moves to a point above another reaction vessel (e.g., 26c) and allow it to discharge the liquid into the latter vessel.
- the other is to take up the nozzles 29, 30 of the pipetter 29 and dispenser 24 from the reaction vessel and move the group of reaction stepwise by drives in the direction indicated by an arrow- (that is, from the positions shown in FIG. 3 to those in FIG. 4).
- the reagent 22 can be added to the sample 21 by means of the dispenser 24 and the chemical reaction time can be controlled by adjusting the time intervals for the horizontal movement of the pipetter nozzle 29 or for the movement of all the reaction vessels.
- a chemical treatment is carried out with the sample retained in a reaction vessel and the transfer of the sample is accomplished by moving the vessel containing the same.
- Flg. schematically represents the concept of the third method known in the art in which a sample is conveyed gravitationally by natural dropping.
- Reaction tanks 48, 49 are communicated to each other by pipes 50, 51 open in the respective tanks, with a valve 53 for shutoff purpose installed between the two pipes.
- the tanks 48, 49 are formed with vents 57, 58, which are open in the atmosphere.
- a sample storage tank 56 is communicated to the upper part of the reaction tank 48 with pipes 52, 55, which are open in the respective tanks and are separated by a valve 54 installed midway.
- a dispenser 43 is operatively connected to valves 44 to enable the reagent 41 from a reagent bottle 47 to flow into the reaction tank 48 via pipes 45, 46.
- Opening the valve 54 allows the sample to run down gravitationally, at a controlled rate, into the reaction tank 48 through the pipes 52, 55. Meanwhile a given quantity of the reagent 41 is added to the sample in the reaction tank 48 by means of the dispenser 43, the addition being followed by a certain waiting period.
- the method of transporting a sample in the apparatus for chemical treatments in accordance with this invention is to convey the sample by controlling the atmosphere surrounding the same, that is, by changing it pressure to atmospheric, positive or negative one.
- numerals 61, 73 indicate reaction tanks wherein sample mixtures are retained and subjected to chemical treatments. They are equipped with auxiliary means so that they can perform practically analogous functions.
- sample lines 62, 74 In the upper parts of the reaction tanks 61, 73 are open sample lines 62, 74, the other ends of which are connected to sampleline valves 63, 75 for opening and closing the lines.
- Sample-drain pipes 64, 76 are open in the lower parts of the reaction tanks 61, 73 and, on the other ends of these pipes, sample-line valves 65, 77 and waste-liquid line valves 72, 84 are installed as shown.
- the sample-line valves 65, 75 are connected via sample pipe 741.
- One end of each of manifolds 66, 78 is open in the upper parts of the reaction tanks 61, 73.
- sample-reagent mixture 42 is conveyed by gravity through the pipe 50, valve 53, and pipe 51 into the lower reaction tank 49.
- This third method is characterized by the retention of the sample in a vessel during its chemical treatment and by the dependence upon natural downflow by gravity for the transport of the sample and the like, which eliminates power requirement.
- a variety of samples cannot be smoothly handled.
- Each border of each reaction tank or the like requires a valve. To reduce the resistances of the pipes and valves is of value in facilitating the transport of the sample but brings a penalty of increased dead space, which in turn may cause undesirable intermingling of different samples when they are to be analyzed in succession.
- reaction tanks 61, 73 equipped with the groups of pipes and valves above described constitute closed reaction tank units 501, 502, respectively.
- a sample pipe 85 is connected to the sample-line valve 63 and is in communication with a sample reservoir (not shown) at the atmospheric pressure or an increased pressure.
- Atmospheric-pressure pipes 86a, 86b are preferably open in the atmosphere through filters or are communicated with an inert-gas reservoir (not shown) at the atmospheric pressure, because the reaction tank units form closed systems.
- Increased-pressure pipes 87a, 87b are likewise in communication through filters to a clean-air or inert-gas source (not shown) under pressure (positive pressure) of 0.0ll kg/cm G.
- Reduced-pressure pipes 88a, 88b are connected to a reduced-pressure (negative pressure) source (not shown), desirably at a pressure between 0.01 and 0.5 kg/cm G.
- Waste-liquid pipes 89a, 89b communicate with a suction source (not shown) at a pressure between 0.01 and 0.5 kg/cm G, which constantly draws up by suction the liquid or gas that flows through the pipes.
- Transference of the sample from the reaction tank 61 to the tank 73 may be accomplished in either of twc ways.
- One is to enable the reaction tank 73 to have a passive function (after which the procedure is hereinaf ter called the passive transference).
- the increased-pressure line valve 68, sample-line valves 65, 75, and atmospheric-pressure line valve 79 are opened. Now that the sample-line valves between the two reaction tanks are open, the sample-line is open, too, and the sample in the reaction tank 61 is forced down into the reaction tank 73 by the increased pressure (positive pressure) being exerted from the above liquid level in the tank 61.
- the sample admitted into the reaction tank 73 is, of course, kept at the atmospheric pressure.
- the other procedure is to permit the reaction tank 73 to have an active function (hereinafter called the active transference).
- the active transference This time the atmospheric-pressure line valve 67, sample-line valves 65, 75, and reduced-pressure line valve 81 are opened. Communication is thus established between the two reaction tanks and, because the pressure in the tank 73 is reduced (negative) whereas the sample in the tank 61 is at the atmospheric pressure, the sample is conveyed from the tank 61 to 73. If the passage and conditions for the conveyance of the sample are the same as in the passive transference, then a negative pressure of about 0.1 kg/cm applied to the reduced-pressure pipe 88b will be sufficient to effect the conveyance.
- the passive transference to the reaction tank 73 means the active transference from the tank 61 and vice versa. Therefore, the afore-described method of supplying the sample to the reaction tank 61 with the reduced-pressure line valve 69 opened corresponds to the active transference to the tank 61.
- the pressure in the vessel after the supply of the sample is kept positive or negative for an excess period of time, so that any sample that may have adhered to the surrounding wall of the passage is blown off clearly by the stream of air or inert gas. Consequently there is no possibility of undesirable intermingling of different samples along any relatively long passage. This is another major advantage of the transference by this procedure.
- the increased-pressure line valve 80 and sampleline valve 77 have only to be opened in order that the reaction tank 73 may accomplish the active transference. If any waste material is to be delivered out for abandonment from either the reaction tank 61 or 73, it is merely necessary to open the waste-liquid line valve 72 or 84 and atmospheric-pressure line valve 67 or 79 as the case may be, and then drain the waste material into the waste-liquid line 89a or 89b which is ready to draw in the waste by suction. As an alternative to this passive transference for the either tank, the active procedure may be resorted to by opening the waste-liquid line valve and increased-pressure line valve of the particular tank.
- the reaction tank units 501, 502 are provided with reagent lines (not shown) through which and the reagent inlet valves 71, 83 a reagent or reagents can be supplied from reagent bottles.
- the reagent or reagents can be added to the samples in the tanks by the passive or active transference and with the use of the reagent inlet valves 71, 83. This, when combined with the contollability of the length of time for which the sample is retained in either reaction tank or the both, will provide the basis for automatization of treatments for chemical analyses.
- the sample pipe 741 if out off midway, will provide two identical reaction tank units 501, 502.
- Each of these units comprises a reaction tank, a sample pipe (for sample feeding) and a valve installed on the upper part of the tank, a sample pipe (for sample discharging) and a valve on the lower part, and a group of valves and lines provided above the vessel to make the pressure therein positive, atmospheric, or negative for the purpose of sample conveyance.
- these reaction tank units as unit equipments each combining active and passive functions, it follows that the units can be connected both in series and parallel. Any unit equipment may be disconnected from, or may be added to, any of complex combinations of unit equipments, without affecting the function of the original combination and that of the automatic controls including the valves.
- a first reaction tank unit 503 like the tank units already described, comprises a reaction tank 91, sample pipe 92, sample-line valve 93, sample-drain pipe 94, atmospheric-pressure line valve 95, increasedpressure line valve 96, reduced-pressure line valve 97, and waste-liquid line valve 98.
- reaction tank units 501, 502 differs from the reaction tank units 501, 502 in that the sample-drain pipe 94 is not terminated with a sample-line valve but is connected to a tee 116.
- Second and third reaction tank units 504, 505 are quite similar to the units 501, 502 shown in FIG. 6. Smaple-line valves 103a, l03b of these reaction tank units are communicated with a tee 117, so that the tank units 504, 505 are on equal terms with the first unit 503.
- a fourth reaction tank unit 506 comprises a reaction tank 108, sample pipe 109, sample-line valve 111, atmospheric-pressure line valve 112, increased-pressure line valve 113, reduced-pressure line valve 114, and waste-liquid line valve 115.
- the sample pipe 109 communicates to the tee 117 instead of a sample-line valve.
- the tee 117 is in communication with the sample-line valves 103a, 103b.
- the second reaction tank unit 504 and the third unit 505 are disposed between and in parallel to the first and fourth units 503, 506. Description of the pipe groups and external supply sources will be omitted hereinafter because, unless otherwise stated, they are in essence the same as those already described in connection with the fundamental principle of this invention.
- the treating time required for the first or third step is a half of the period for the second step.
- the reaction tank units are desirably connected as illustrated in FIG. 7. Unless otherwise stated, all valves are construed to remain closed.
- the sample is introduced into the reaction tank unit 503 by the active transference, that is, by opening the sample-line valve 93 and reducedpressure line valve 97 and thereby reducing the pressure in the tank 91.
- the atmospheric-pres sure line valve 95 is once opened to increase the pressure of the sample to the atmospheric level, and then the first-step chemical treatment is carried out.
- the sample is transferredto the second reaction tank unit 504.
- the transference may be accomplished in either of two ways.
- One method is, in this case, the passive transference to the reaction tank unit 504, whereby the increased-pressure line valve 96, sample-line valve 101a, and atmospheric-pressure line valve 104a are opened to place the sample inside the reaction tank 91 under an increased pressure.
- the other is the active transference to the same unit 504 whereby the atmospheric-pressure line valve 95, sampleline valve 101a, and reduced-pressure line valve 106a are opened.
- the atmospheric-pressure line valve is once opened to maintain the pressure in the vessels at the atmospheric level.
- the second-step chemical treatment is effected.
- the first reaction tank unit 503 is allowed to repeat the first-step treatment with another sample while, at the same time, the second step is in progress.
- the first sample is then transferred to the third reaction tank unit 505 in the same manner as when it was conveyed from the first unit 503 to the second 504, except that the sample-line valve 10111 is employed this time.
- the second-step treatment is repeated.
- the method of sample transference is limited to one, passive or active, depending upon the type of unit equipment to be employed for a particular chemical treatment or upon the type of sample or reagent to be handled.
- the sample is then transferred from the second reaction tank unit 504 to the fourth unit 506. Again, two alternatives are open.
- the other is the active transference whereby the atmospheric-pressure line valve 104a, sample-line valve 103a, and reduced-pressure line valve 114 are opened for the conveyance purpose.
- the increased-pressure line valve 113 and sample-line valve 111 are opened and, by this active transference from the unit 506, the sample is transferred elsewhere.
- reaction tank units for parallel connection
- more reaction tank units may be connected in parallel or, as a further alternative, groups of serially connected units may be connected altogether in parallel.
- reaction tank units have been regarded as components of a unit equipment. Now that equipments having separate functions of chemical treatments will be considered.
- a sample pipe 132 is open in the upper part of a reaction tank 131 and is connected at the other end to a sampleline valve 133.
- a sample-drain pipe 134 which is open in the lower part of the reaction tank 131 is communicated with a sample-line valve 135 and a waste-liquid line valve 141.
- a manifold 136 which is open in the upper part of the tank communicates to an atmosphericpressure line valve 137, an increased-pressure line valve 138, and a reduced-pressure line valve 139.
- this unit 507 will be described later hereunder.
- the description of the lines and external supply sources required for the operation will be omitted because they are essentially the same as those which have already been described.
- all valves are normally closed and the reaction tank or other vessel to be described later is hermetically sealed. The same applies to all of the equipments to be described later and, therefore, these provisos will be omitted for brevity from the the following description.
- the sample-line valve 133 and atmosphericpressure line valve 137 or reduced-pressure line valve 139 are opened to admit the sample into the reaction tank 131 by the passive or active transference to the reaction tank unit 507.
- the atmospheric-pressure line valve 137 is opened for some time to maintain the sample at the prevailing atmospheric pressure.
- the valves 142 operatively connected to the dispenser 143 are manipulated, so that a given amount of the reagent can be added to the sample by way of the reagent pipe 140. This may be effected, if necessary,
- a valve such as indicated at 71 in FIG. 6 may be employed provided that the given amount of the reagent can be measured into the tank by some suitable means.
- the valve to be used must be capable of hermetically closing the reagent-addition unit, even on a temporary basis. Also it should be clear that, while one type of reagent is handled in the unit being described, many different reagents may be added, instead, in a similar way.
- the atmospheric-pressure line valve is closed and agitation is discontinued.
- either the passive or active transference from the reaction tank unit 507 is effected by opening the sample-line valve 135 and atmosphericpressure line valve 137 or increased-pressure line valve 138. If useless sample is to be discarded, the waste-liquid line valve 141 is used in lieu of the sample-line valve 135.
- a sample-line valve 153 is installed in communication with a sample pipe 152, which in turn is open in the upper part of a container 151.
- a sample-drain pipe 154 open at one end in the lower part of the container 151 is communicated at the other end with a sample-line valve 155 and a waste-liquid line valve 159.
- a manifold 156 which is open in the upper part of the container 151, there are installed an atmospheric-pressure line valve 157 and an increased-pressure line valve 158.
- a nozzle 160 is open in a suitable position inside the container via a gastight seal (not shown) capable of moving up and down in the upper part of the vessel.
- the other end of the nozzle communicates to a line 162 through a valve 161.
- a line 162 Such is the construction of a fixed-quantity sampling unit 508.
- the line 162 inside of which is kept at a reduced pressure by some suitable means, attracts fluid, either liquid or gas.
- this fixed-quantity sampling unit 508 will now be explained.
- the sampleline valve 153 and valve 161 are opened first. This results in a reduced pressure inside the container 151, and the sample begins to be conveyed through the pipe 152 into the vessel.
- any excess of the sample is drawn up by suction into the line 162 through the nozzle 160 and valve 161, with the consequence that the liquid level of the sample 163 is kept constant.
- the excess sample will be taken up by the nozzle 160 when the sample-line valve 153 is closed while, at the same time, the atmospheric-pressure line valve 157 is opened. As a result, the liquid level of the sample 163 will be maintained constant.
- the opening position of the nozzle 160 may be preset so that a predetermined amount of the sample 163 can be held within the container.
- the method is tantamount to the active transference to the sampling unit 508.
- the measured amount of the sample 163 is either transferred to some other place or abandoned by the active transference from the unit by opening the increasedpressure line valve 158 and sample-line valve or waste-liquid line valve 159.
- This fixed-quantity sampling unit may be utilized to collect the supernatant fluid from a solution containing sediments, in which case the opening position of the nozzle has only to be chosen so that the portion of the liquid which tends to be relatively easily clarified can be collected.
- the third example of unit equipment is a dilution unit, either of a photoelectric type or an electric conductivity type, as schematically represented in FIG. 10 or 11, respectively.
- the unit shown in FIG. 10 will be described first.
- a sample pipe 172 which is equipped with a sample-line valve 173.
- a sample-drain pipe 174 which in turn communicates to a sample-line valve 175 and a waste-liquid line valve 182.
- a manifold 176 open at one end in the upper part of the tank 171 is also in communication with an atmospheric-pressure line valve 177, an increased-pressure line valve 178, and a reduced-pressure line valve 179.
- a reagent pipe 180 extends downward through a valve 181 and opens in the reaction tank 171. Further, along both sides of the tank there are located a light source 183 and a light-beam detector 184, in positions opposite to each other and in such a way that they can be moved up and down by some suitable means (not shown) with respect to the tank 171. Signals from the light-beam detector 184 are sent to a controller 185, so that the sample-line valve 181 can be opened or closed depending upon the presence or absence of the detection signals.
- a controller 185 Such is the construction of a dilution unit 509.
- the unit is operated in the following manner. It is assumed that the reaction tank 171 is filled with a given quantity of sample by the procedure already described in connection with the reagent-addition unit, and that the sample is to be diluted, for example, with water.
- the light source 183 and light-beam detector 184 are located on a level equal to that of the liquid after dilution.
- the optical instrument of this type detects the deflection of the path of a light beam from the source 183 due to the difference between air and the sample (liquid), in terms of ON-OFF signals on the detector 184.
- the controller 185 is so adjusted that, when there is a predetermined amount of the sample in the reaction tank 171, the valve 181 is kept open and the reagent (mere water in this case) is allowed to drop from the bottle 186 into the reaction tank 171 until the liquid level of the sample in the tank comes up to the light path.
- the reagent or water is added only when there is a predetermined amount of the sample in the reaction tank or, in other words, dilution to a predetermined level is accomplished.
- the errors in dilution were in the range of plus or minus 0.2% per 100 ml of the diluted solution.
- the arrangement shown in FIG. 11, or the electric conductivity type, differs from the type of FIG. 10 in the method of detecting the liquid level after the dilution as specified.
- the type of FIG. 10 detects the level optically, whereas that of FIG. 11 detects it by means of an electrode that forms a part of an electric circuit.
- a controller 204 comprises the electric circuit including the electrode 203 as one of its components, and functions so that, when there is the sample to be diluted in the reaction tank 191, the controller cooperates with the electric circuit to open a reagent inlet valve 201 and admit the reagent (e.g., water) into the reaction tank and, when the liquid level of the diluted sample has reached the electrode 203, it closes the reagent inlet valve 201.
- a reagent inlet valve 201 admit the reagent (e.g., water) into the reaction tank and, when the liquid level of the diluted sample has reached the electrode 203, it closes the reagent inlet valve 201.
- the electric circuit is used to detect the difference between the electric conductivities of the air and the sample between the element wires of the electrode 203.
- the circuit is of the electric conductivity type.
- the components described above are assembled to form a dilution unit 510.
- the electric conductivity system of the dilution unit 510 works in the manner now to be described. It is assumed that the reaction tank 191 is prefilled with a given amount of the sample and that the sample is to be diluted to a certain volume with the addition, for example, of water.
- the electrode 203 is installed at the height corresponding to the liquid level after the dilution.
- the controller 204 opens the reagent inlet valve 201 in response to a signal from the outside, so that the reagent (or water in this case) is admitted into the reaction tank 191. If necessary, the sample may be agitated by an agitator (not shown).
- the controller 204 closes the sample inlet valve 201, thus completing the dilution.
- the accuracy of dilution with this unit 510, as well as with a dilution unit of a high-frequency transmission type was less than plus or minus 0.2% for the sample volume of 100 ml, where a reagent inlet pipe 200 having an inside diameter of 2.4 mm was employed.
- Dropwise introduction of the reagent into the reaction tank 171 may be effected in two ways; either by opening'only the atmospheric-pressure line valve 177 and allowing the reagent to flow down by gravity, or by opening only the reduced-pressure line valve 179 and thereby reducing the pressure in the reaction tank 171.
- the fourth example of unit equipment is a washing unit, as schematically shown in FIG. 12. It is more practical to employ this washing unit as a washer for a reaction tank or container of another unit equipment than to consider it as a unit equipment. However, for the simplicity of explanation, it is taken here as an independent unit equipment. It will be seen from the foregoing description about the three different unit equipment that those units have many parts in common. The illustration and description of the common parts do not appear essential for the explanation of the functional principles of the unit equipments and, therefore, will be omitted hereinafter.
- this washing unit 511 and the washing method adopted will be described below.
- the inner wall of the reaction tank 211 is assumed to be contaminated.
- the washing operation can be carried out in a number of ways.
- the waste-liquid line valve 213 and atmospheric-pressure line valve 215 are opened to allow the contaminant to drain from the reaction tank 211 into the waste-liquid line (not. shown) wherein the partial vacuum continues to provide suction as well as in the reaction tank.
- the change-over valve 219 is manipulated (to the position in FIG. 12) where it communicates the washing nozzle 217 to the washing-solution A line 220 at an increased pressure or at the prevailing atmospheric pressure.
- the washing solution A introduced through the washing nozzle 217 is then scattered by the sprinkler 218 to wash the inner wall surface of the reaction tank and flow down into the waste-liquid line (when, if necessary, the atmospheric-pressure line valve 215 may be closed.)
- the wasteliquid line valve 213 is closed and the atmosphericpressure line valve 215 is opened so that the washing solution A under pressure or at the atmospheric pressure can be led through the change-over valve 219 and collected in the reaction tank 211.
- the washings are allowed to drain in either of two ways.
- the waste-liquid line valve 213 and atmospheric-pressure line valve 215 are opened and the washing are caused to flow down into the waste-liquid line wherein the suction still prevails. Or, the atmospheric-pressure line valve 215 is closed and the increased-pressure line valve 216 and waste-liquid line valve 213 are opened to flow down the washings. If the washing solution A alone cannot wash well, the change-over valve 219 may be manipulated to use the washing solution B, too.
- three or more different washing solutions may be used in this manner. For example, in the case of the hydroxides in river water that precipitate on the alkaline side of pH 10 in a reaction tank capable of treating ml of the sample, mere distilled water cannot thoroughly wash the deposits away. It is customary in such occasion to dissolve the deposits with a dilute acid and then wash away the acidic solution with distilled water. In this manner thorough washing is accomplished.
- the fifth, of unit equipments is hydrogen-ion-concentration (pH)-adjusting unit.
- FIG. 13 illustrates the unit schematically.
- pH adjustment usually a commercially available pH meter equipped with an automatic titrator is used.
- a com-dion-concentration (pH)-adjusting unit usually a commercially available pH meter equipped with an automatic titrator is used.
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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JP9173172A JPS5311238B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) | 1972-09-14 | 1972-09-14 |
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US3929411A true US3929411A (en) | 1975-12-30 |
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ID=14034643
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US39229473 Expired - Lifetime US3929411A (en) | 1972-09-14 | 1973-08-28 | Sample transfer device and method for analytical system |
Country Status (4)
Cited By (46)
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US4113437A (en) * | 1975-08-13 | 1978-09-12 | The Secretary Of State For Social Services | Liquid storage device |
FR2389125A1 (fr) * | 1977-04-26 | 1978-11-24 | Bodenseewerk Perkin Elmer Co | Appareil a former et a transferer un echantillon gazeux de mesure |
US4138215A (en) * | 1976-06-18 | 1979-02-06 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Method and apparatus for generating and transferring a gaseous test sample |
US4230665A (en) * | 1977-07-01 | 1980-10-28 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Apparatus for automatically generating and measuring gaseous measuring samples from a series of liquid samples |
US4268478A (en) * | 1976-06-18 | 1981-05-19 | Bodenseewerk Perkin-Elmer & Co. Gmbh | Method and apparatus for generating and transferring a gaseous test sample |
US4273742A (en) * | 1978-11-25 | 1981-06-16 | Bodenseewerk Perkin-Elmer | Drain apparatus for the reaction vessel in an atomic absorption instrument |
US4503012A (en) * | 1983-04-19 | 1985-03-05 | American Monitor Corporation | Reagent dispensing system |
US4632808A (en) * | 1983-04-15 | 1986-12-30 | Science And Technology Agency | Chemical manipulator |
US4769217A (en) * | 1985-04-29 | 1988-09-06 | Servomex Company | Apparatus for measuring content of organic carbon |
US4818706A (en) * | 1983-04-19 | 1989-04-04 | American Monitor Corporation | Reagent-dispensing system and method |
US4925628A (en) * | 1986-12-16 | 1990-05-15 | Ciba-Geigy Corporation | Sample preparation chamber with mixer/grinder and sample aliquot isolation |
US4980130A (en) * | 1986-12-16 | 1990-12-25 | Ciba-Geigy Corporation | System for preparation of samples for analysis |
US5254311A (en) * | 1991-07-02 | 1993-10-19 | Olympus Optical Co., Ltd. | Continuous multinominal analysis method and apparatus |
US5470540A (en) * | 1990-12-14 | 1995-11-28 | Bp Chemicals Limited | Apparatus and process for introducing a suspension into a reactor |
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US5826631A (en) * | 1984-11-08 | 1998-10-27 | Earth Resources Corporation | Cylinder rupture vessel |
US5849598A (en) * | 1996-03-15 | 1998-12-15 | Washington University | Method for transferring micro quantities of liquid samples to discrete locations |
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Cited By (60)
Publication number | Priority date | Publication date | Assignee | Title |
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US4113437A (en) * | 1975-08-13 | 1978-09-12 | The Secretary Of State For Social Services | Liquid storage device |
US4138215A (en) * | 1976-06-18 | 1979-02-06 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Method and apparatus for generating and transferring a gaseous test sample |
US4268478A (en) * | 1976-06-18 | 1981-05-19 | Bodenseewerk Perkin-Elmer & Co. Gmbh | Method and apparatus for generating and transferring a gaseous test sample |
FR2389125A1 (fr) * | 1977-04-26 | 1978-11-24 | Bodenseewerk Perkin Elmer Co | Appareil a former et a transferer un echantillon gazeux de mesure |
US4208372A (en) * | 1977-04-26 | 1980-06-17 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Apparatus for generating and transferring a gaseous test sample to an atomic absorption spectrometer |
US4230665A (en) * | 1977-07-01 | 1980-10-28 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Apparatus for automatically generating and measuring gaseous measuring samples from a series of liquid samples |
US4273742A (en) * | 1978-11-25 | 1981-06-16 | Bodenseewerk Perkin-Elmer | Drain apparatus for the reaction vessel in an atomic absorption instrument |
US4632808A (en) * | 1983-04-15 | 1986-12-30 | Science And Technology Agency | Chemical manipulator |
US4735776A (en) * | 1983-04-15 | 1988-04-05 | Science And Technology Agency | Chemical manipulator |
US4818706A (en) * | 1983-04-19 | 1989-04-04 | American Monitor Corporation | Reagent-dispensing system and method |
US4503012A (en) * | 1983-04-19 | 1985-03-05 | American Monitor Corporation | Reagent dispensing system |
US5826631A (en) * | 1984-11-08 | 1998-10-27 | Earth Resources Corporation | Cylinder rupture vessel |
US4769217A (en) * | 1985-04-29 | 1988-09-06 | Servomex Company | Apparatus for measuring content of organic carbon |
US4925628A (en) * | 1986-12-16 | 1990-05-15 | Ciba-Geigy Corporation | Sample preparation chamber with mixer/grinder and sample aliquot isolation |
US4980130A (en) * | 1986-12-16 | 1990-12-25 | Ciba-Geigy Corporation | System for preparation of samples for analysis |
US5470540A (en) * | 1990-12-14 | 1995-11-28 | Bp Chemicals Limited | Apparatus and process for introducing a suspension into a reactor |
US5254311A (en) * | 1991-07-02 | 1993-10-19 | Olympus Optical Co., Ltd. | Continuous multinominal analysis method and apparatus |
US5527507A (en) * | 1992-10-01 | 1996-06-18 | American Sterilizer Company | Accumulator based liquid metering system and method |
US6240981B1 (en) | 1993-05-28 | 2001-06-05 | Earth Resources Corporation | Apparatus and method for controlled penetration of compressed fluid cylinders |
US5510018A (en) * | 1993-11-30 | 1996-04-23 | Danieli & C. Officine Meccaniche Spa | System to re-circulate treatment material in processes of surface treatment and finishing |
US6267931B1 (en) | 1994-02-03 | 2001-07-31 | Earth Resources Corporation | Reconfigurable waste treatment system |
US5723093A (en) * | 1994-07-19 | 1998-03-03 | Commissariat A L'energie Atomique | Apparatus for the continuous sampling and analysis of a liquid effluent |
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Also Published As
Publication number | Publication date |
---|---|
JPS4950985A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) | 1974-05-17 |
JPS5311238B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) | 1978-04-20 |
GB1439483A (en) | 1976-06-16 |
DE2346203A1 (de) | 1974-04-25 |
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