US3401564A - Apparatus for transferring measured samples - Google Patents

Apparatus for transferring measured samples Download PDF

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Publication number
US3401564A
US3401564A US550828A US55082866A US3401564A US 3401564 A US3401564 A US 3401564A US 550828 A US550828 A US 550828A US 55082866 A US55082866 A US 55082866A US 3401564 A US3401564 A US 3401564A
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United States
Prior art keywords
tube
sample
tubing
samples
capillary
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US550828A
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English (en)
Inventor
Hrdina Jiri
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Czech Academy of Sciences CAS
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Czech Academy of Sciences CAS
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02—Burettes; Pipettes
    • B01L3/021—Pipettes, i.e. with only one conduit for withdrawing and redistributing liquids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/24—Automatic injection systems

Definitions

  • An arrangement for transferring dosed samples, particularly for automatic analyzers which includes at least one sample tube; a distributing valve; a discharge tubing; means for connecting one end of said sample tube with said distributing valve while the other end of said sample tube is adapted to be connected with said discharge tubing; means for sealing the connection between said other end of the sample tube and the discharge tubing and means for imparting a relative movement between the second end of the sample tube and the discharge tubing so as to allow alternately free access to this other end of the sample tube, and to accomplish a tight coupling between the sample tube and the discharge tubing.
  • This invention relates to an arrangement for transferring dosed samples of liquids, especially mixtures of substances designed for analyses in automatic analyzers.
  • an important partial unit is a device which will permit dosed samples designed for anaysis to be individually and subsequently at the beginning of every analysis transferred to columns or in general to places of their processing.
  • an important requirement is that the samples be transferred automatically to columns with minimum undesirable debasement of the partition which is provided by the column. It is necessary to suppress as much as possible the blurring of zones caused by the decrease of concentration gradients in consequence of mixing with neighboring liquids on storing of samples in recipients and transferring them to the column.
  • the sample recipient at the time of dosing must be easily disconnectable from the capillary tubing leading to the column in such way that the filling of the samples into the sample recipients may be carried out comfortably, accurately and with minimum danger of a part of 3,401,564 Patented Sept. 17, 1968 the sample adhering to undesirable places from where they would not at the time of beginning of the analysis get to the column.
  • the arrangement according to the invention fulfills all the above-given conditions together with advantage of comparative simplicity, reability and especially simple operation.
  • the arrangement according to the invention is essentially formed by at least one sample tube which can be connected tightly into the circuit of the main pump of the analyzer, which tube is 'by one of its en-ds connected to the tubing leading to a hydraulic switch which permits the tube to be connected both to the source securing the inflow of the liquid which causes the dispensing of the sample from the tube to the place of processing and to a suction tubing for sucking on the sample from a sample reservoir, the free end of the sample tubes being preferably adapted to be released and to be inserted into holders in which the inlet and the outlet tubings terminate, which are connected in a through-flow manner with the free end of the tube.
  • One of the ends of the sample tube preferably the upper one, is purposefully firmly connected to a flexible hose, and the other one, preferable the lower one, is connected to a tubing so that the connection can be disconnected; this tubing may lead to a column via a further distributor valve and tubing.
  • FIG. 1 is a vertical section of one of the sample recipients together with a device securing a releasable sealmg.
  • FIG. 2 shows in cross section the connection of the flexible hose to a connecting body
  • FIG. 3 is a side view upon the carrier of a spring
  • FIG. 4 is a top view upon the lever, on which the sample tube is suspended.
  • FIG. 5 is a cross section of the lower part of the sample tube and of its connection with the discharge tubing.
  • FIG. 6 represents another version with a zig-zag bent sample recipient.
  • FIG. 7 shows an example of a general arrangement with more sample recipients connected into the pressure branch of a pump forcing the eluents to chromatographic columns.
  • FIGS. 1 to 5 show the sample recipients used in the device in the shape of thick-walled glass capillary tubes 1 which are narrowed at their bottom end 2.
  • the upper end of the tube 1 is connected to a flexible inlet hose 3 which need not be a capillary one.
  • a connecting body 5 for example of stainless steel; the hose 3 is at its lower end 6 flared and sealed by the thrust of a hollow sealing screw 7 which acts via a ring 8 on a sealing ring 9 of silicon rubber.
  • the connecting body is suspended by means of a pivot 10 to a lever 11 swinging round a pivot 12 mounted in a cutout of a plate 13 fastened to the base plate 14.
  • the lever 11 is at its left end provided with a handle 15, at the right end with a cut-out 16 through which passes a screw 17 provided with a nut 18 for limiting the motion of the right end of the lever 11 on which acts in the direction of the arrow 19 the force of a spring 20 centered by discs 21 and 22 round the screw 17 mounted by its lower end into an angle 23 fastened by screws 24 to the base plate.
  • the stress of the spring 20 may be adjusted after loosening of the screws 24 by a vertical motion of the angle carrier 23, for which purpose the carrier 23 has vertical adjusting cut-outs 25 for the fastening and adjusting screws 24.
  • the nut 18 on the screw 17 limits the motion of the right end of the lever 11 in the upward direction under pressure of the spring 20 in such way that this limiting is also effective in case the tube 1 does not rest on the lower sealing supports, i.e., for example in case the tube 1 is for the purpose of filling deviated from the vertical position shown by full lines to the position 101 drawn by a dashed line.
  • the tube 1 after releasing of the lower connection, is forced by a small force of a fiat pressure spring 26 mounted to the base plate 14 by a screw 27.
  • position 1 drawn by a dashed line it is possible to suck into the tube 1 the sample and other liquids including bubble pistons.
  • sample tubes 1 When the sample tubes 1 are not being filled, they are in position 1, drawn by a full line, where they rest under the pressure of the spring 20, transmitted by the lever 11, on a culfpacking 30 of an elastic and chemically inert material, for example silicon rubber.
  • the cuff 30 is tightly mounted into a packing body 31 into which engages a hollow needle 32 on whose lower end is tightly slid an outlet capillary 33.
  • the packing body 31 is clamped and centered by a bore 34 in the body 35 mounted by connecting screws 351 to the base plate 14.
  • the needle 32 may pass through the central hole of the cuffpacking 30 and possibly even overhang as far as to the narrowed lower opening of the lower end 2 of the tube 1.
  • the hollow needle 32 may reach as far as to the capillary cavity of the lower end 2 of the tube 1.
  • the transmitted force of the spring 20 should not cause crushing or some other damage of the lower narrowed end 2 of the tube 1 or even on the upper end of the hollow needle 32, it is necessary to secure with a relatively great accuracy a sufficiently centric mounting of the lower end 2 of the tube 1 on the cuffpacking 30 and the upper end of the hollow needle 32.
  • This is secured by the cylindrical portion 36 of the cavity of the packing body 31 being precisely centric with the hollow needle which is pressed into the hole in the lower portion of the packing body 31.
  • the cavity 36 enlarges conically in the upper portion of the packing body 31.
  • the tube 1 is centered roughly in addition by being, after completion of a filling and with the handle 15 of the lever 11 lifted manually against the force of the spring 20, introduced into the cut-out 38 of the angle 39 fastened by a screw 40 to the base plate 14.
  • This preliminary centering takes place automatically simply by the pressure of a finger in the direction of the arrow against the force of the spring 26, bringing the tube 1, which will enter the centering cut-out 38 of the angle 39, to a position where further precise guidance is provided by the surfaces 37 and 36 of the packing body 31, as the tube 1 is lowered under the transmitted pressure of the spring 20, in case the manual action on the handle 15 of the lever is released.
  • the position of the stop nut 18 is so selected that upon full bearing of the lower end 2 of the tube 1 on the elastic cuff 30 the pressure of the spring 20 may not be eliminated by the hearing of the right end of the lever 11 on the limiting nut 18.
  • the tube 1 as shown in FIG. 1 can remain permanently stable on the other hand the parts mounted to the plate 14, especially the packing body 31 and the elements connected with it can be moved.
  • the same functional relative positions of the tube 1 and the packing body 31 towards each other can be accomplished.
  • Both the above and a number of further possible alternatives permit a perfectly tight connection of the sample tube 1 with the tubings, the lower joint being from the point of view of manipulation easily disconnectable for the purpose of filling.
  • the tube 1 may even at greater lengths be dimensioned so as to have a sufficient strut strength.
  • the narrowing of the tube 1 at the lower end is such that on the one hand it does not decrease the strut strength and on the other hand it helps accomplish a great specific pressure on the cuff 30 as it is necessary for a. perfect sealing.
  • the narrowed lower end 2 provides a substantially smaller outer surface which is wetted by the sample or by other liquids on filling.
  • a sample tube 1 of greater length can hold more than one sample with the possibility of each sample being separated from the other ones by means of bubble pistons.
  • the adverse effect of the bubble pistons on the function of a column is practically obviated by the bubble remaining above the upper filling of the column and dissolving in a short time by the action of a deaerated eluent, especially in that case when the bubble is scattered into many small bubbles on passage through a porous body, which effect is used in modern closures of chromat-ographic columns.
  • the device according to the invention fulfills optimally the conditions of automatic introduction of samples to columns even under difficult conditions given especially by high pressures which occur in especially effective modern methods of chromatographic and similar analyses. But it can also be used even for other purposes, for example for automatic introduction of samples to columns via a pump designed for pumping of eluents. In this case the device is placed in the suction branch of the pump.
  • the conditions of operation are here substantially simpler, especially because the pressure action here is unnecessary.
  • FIG. 6 exemplifies schematically a version using a long sample tube 102, once or several times bent.
  • sample tube 102 may be bent several times and clamped not by its upper end but near its lower end 2 by means of grips.
  • a design is represented where the sample tube 102 is bent twice and held near its lower end by two grips 43 and 44 fixed to the base plate 14. In order to secure that the tube 102 will not slip through the grips, it may have one or more lugs 45 fixed thereto.
  • the design according to FIG. 6 is an example of the above-given second possible version where the tube 1 is stable and movable are on the contrary the parts that secure a tight connection of the lower end of the tube with the outlet capillary 33.
  • the members marked with the same reference marks have the same function and significance as in FIGS. 1 to 5.
  • the lever 11 according to FIG. 6 can swing round the joint 12 fastened in a holder 46 fixed by means of screws 47 to the base plate 14.
  • a swinging lever 48 for transmitting the force of the spring 20 acting in the direction of the arrow 49 transmits the force by means of a joint 50 to a pull rod 51 on which is mounted a holder 35 which carries the packing body 31 forming in principle the releasable connection with the outlet capillary 33, the sealing proper and the linking of the tubing being identical with the case according to FIGS. 1 to 5.
  • the pull rod 51 swings after release with the parts mounted on it by the effect of a weak spring 26 to position 510 represented by a dashed line.
  • the swing of the pull bar 51 is limited by a stop formed conveniently by an adjustable screw 52.
  • the lever 48 is connected by means of a point 53 to a further lever 54 of the shape represented which passes as well as thelever 48 through a hole in the base plate 14.
  • FIG. 7 An example of connection of the tubes 1 into the pressure circuit is schematically shown in FIG. 7.
  • the sample tubes 1 in a larger number, for example six, are arranged parallel so as to form a battery of tubes 1 represented in FIG. 1 by two tubes.
  • the individual sample tubes 1 are connected by their lower ends subsequently via a multiway distributing valve 55 to the capillary tubing 56 leading to the column 57.
  • the eluent is forced simultaneously into all the sample tubes 1, except the one which is possibly just being filled by means of the pump 58 whose discharge side is connected by means of a tubing 59 to the upper distributing valve 60.
  • This valve 60 is so arranged that normally the tubing 59 communicates by means of a circumferential groove 61 with all individual sample tubes 1 by means of a connecting hose 3. However, flow occurs only through that tube 1 whose outlet tubing 33 is interconnected to tubing 56 by a channel 62 in the spindle of the distributing valve 55.
  • the circumferential groove 61 of the upper valve 60 is interrupted by a bridge 63 in which opens a channel 64. If the spindle of the valve 60 is so turned that the channel 64 communicates with a certain one of the branches 65 to which are connected individual hoses 3, then this branch and the hose and also the respective sample tube 1 are disconnected from communication with the tubing 59 and the pump 58.
  • one of the sample tubes I communicating with the channel 64 which at the same time permanently communicates With the tubing '66, can be filled in such way that, using the above-given manipulations, the connection of the sample tube 1 with the respective outlet capillary 33 is released, whereby filling is accomplished with the lower end of the tube disconnected by suction by means of a suction tubing 66 which through the channel 64 communicates with the respective connecting hose 3 leading to the particular sample tube 1 which is just being filled.
  • An arrangement for transferring dosed samples particularly for automatic analyzers comprising at least one sample tube, a distributing valve, a discharge tubing, means for connecting one end of said sample tube with said distributing valve, the other end of said sample tube adapted to be connected with said discharge tubing, means for sealing the connection between said other end of the sample tube and the discharge tubing and means for imparting a relative movement between the second end of the sample tube and the discharge tubing so as to allow alternately free access to this other end of the sample tube, and to accomplish a tight coupling between the sample tube and the discharge tubing.
  • An arrangement as in claim 1 comprising a spring loaded lever system supporting the sample tube and urging the same into tight connection with said discharge tubing.
  • An arrangement as in claim 1 comprising a spring loaded lever system supporting the discharge tubing and urging the same into a tight connection with said sample tube.
  • An arrangement as in claim 1 comprising a tight connection-made of a yieldable material between the end of the sample tube and the discharge tubing; and a hollow needle passing through said yieldable material, said needle extending into the sample tube and being connected to the discharge tubing.
  • An arrangement as in claim 1 comprising guiding v ,7 References Cited means securing the correct relative position of the sample UNITED STATES PATENTS tube and the discharge tubing.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
US550828A 1965-05-19 1966-05-17 Apparatus for transferring measured samples Expired - Lifetime US3401564A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CS324565 1965-05-19

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US3401564A true US3401564A (en) 1968-09-17

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US550828A Expired - Lifetime US3401564A (en) 1965-05-19 1966-05-17 Apparatus for transferring measured samples

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US (1) US3401564A (de)
AT (1) AT286684B (de)
BE (1) BE681196A (de)
CH (1) CH459608A (de)
DE (1) DE1598267C3 (de)
GB (1) GB1119198A (de)
SE (1) SE316635B (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3501964A (en) * 1968-03-29 1970-03-24 Drummond Instr Co Assembly for injecting liquid samples into the chamber of a gas chromatography apparatus
US4584887A (en) * 1984-10-10 1986-04-29 The United States Of America As Represented By The Administrator Of The National Aeronautics & Space Administration Solid sorbent air sampler
US4621534A (en) * 1983-09-14 1986-11-11 Carlo Erba Strumentazione S.P.A. Automatic sample apparatus, valve and sampling method
US4688436A (en) * 1985-04-19 1987-08-25 Association Pour La Recherche Et Le Developpement Des Methodes Et Processus Industrielles (A.R.M.I.N.E.S.) Automatic pressurized fluid micro-sampling and injection device
US4939943A (en) * 1988-02-11 1990-07-10 Hewlett-Packard Company Sample injector for a liquid chromatograph
US5133218A (en) * 1989-07-24 1992-07-28 Tritech Partners Sample liquid aspirating and dispensing probe
CN116298181A (zh) * 2023-05-16 2023-06-23 山西国新科莱天然气有限公司 一种天然气中硫化物的检测装置

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3104617A1 (de) * 1980-02-12 1982-01-14 List, Hans, Prof. Dipl.-Ing. Dr.Dr.h.c., Graz Analysengeraet zur messung von fluessigkeitsproben und einrichtung zur einstellung eines bestimmten betriebszustandes desselben
DE3917840A1 (de) * 1989-06-01 1990-12-06 Bodenseewerk Perkin Elmer Co Anordnung zur anreicherung von probensubstanz fuer spektroskopische zwecke bei der fliessinjektions-analyse
JP6611398B2 (ja) * 2016-05-17 2019-11-27 株式会社日立ハイテクノロジーズ 分離カラム接続装置、接続方法及び分析システム

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2448206A (en) * 1943-12-29 1948-08-31 Hays Corp Gas analyzer
US2757541A (en) * 1956-02-27 1956-08-07 Perkin Elmer Corp Sampling apparatus

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2448206A (en) * 1943-12-29 1948-08-31 Hays Corp Gas analyzer
US2757541A (en) * 1956-02-27 1956-08-07 Perkin Elmer Corp Sampling apparatus

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3501964A (en) * 1968-03-29 1970-03-24 Drummond Instr Co Assembly for injecting liquid samples into the chamber of a gas chromatography apparatus
US4621534A (en) * 1983-09-14 1986-11-11 Carlo Erba Strumentazione S.P.A. Automatic sample apparatus, valve and sampling method
US4584887A (en) * 1984-10-10 1986-04-29 The United States Of America As Represented By The Administrator Of The National Aeronautics & Space Administration Solid sorbent air sampler
US4688436A (en) * 1985-04-19 1987-08-25 Association Pour La Recherche Et Le Developpement Des Methodes Et Processus Industrielles (A.R.M.I.N.E.S.) Automatic pressurized fluid micro-sampling and injection device
US4939943A (en) * 1988-02-11 1990-07-10 Hewlett-Packard Company Sample injector for a liquid chromatograph
US5133218A (en) * 1989-07-24 1992-07-28 Tritech Partners Sample liquid aspirating and dispensing probe
CN116298181A (zh) * 2023-05-16 2023-06-23 山西国新科莱天然气有限公司 一种天然气中硫化物的检测装置
CN116298181B (zh) * 2023-05-16 2023-07-21 山西国新科莱天然气有限公司 一种天然气中硫化物的检测装置

Also Published As

Publication number Publication date
DE1598267C3 (de) 1974-06-20
DE1598267A1 (de) 1970-12-17
CH459608A (de) 1968-07-15
GB1119198A (en) 1968-07-10
DE1598267B2 (de) 1973-10-18
SE316635B (de) 1969-10-27
AT286684B (de) 1970-12-28
BE681196A (de) 1966-10-31

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