DE7523561U - CAP FOR REACTION VESSEL - Google Patents

Description

EEHRINGVJERKE _{AKTIENGESELLSCHAFT:} MarUirg '{Lahn)

File number: Hoe 75 / B 006 u.H. - Ma 225 Date: July 23, 1975

Closure for reaction vessels

The invention relates to a closure designed as a metering device for reaction vessels. i

For chemical reactions, especially in analytical processes, an exact amount of a substance must often be made available and added to a reaction mixture located in a vessel at the appropriate time. Thus, in series tests which, for example, take place in a two-stage reaction, after the first stage the required reagent _k for the second stage must usually be very laborious, or in series investigations a reaction mixture of several liquid or solid reagents that must be kept separately are added. Not inconsiderable errors must be expected if the reagent is in solid form. There is therefore a need for Vox devices that allow precise dosing of solid, but also liquid substances that have to be added to a reaction medium at a certain time and that can be safely used by unskilled personnel.

The object of the invention is therefore to provide a metering device to create the type in question, which requires little equipment and with the help of a precise dosed amount of a solid or liquid. Substance can be stored and delivered. This object is achieved according to the invention solved that the vessel closure is designed as a metering device.

, 7523561 01/26/78

*. '. ·: I ... "Ma 225

The invention therefore relates to a device for locking for vessels and for storing and dispensing a dosed amount of a solid or liquid substance, characterized in that, that an elastic cap closure is replaced by a removable one Plate has to be sealed interior space with a centrally arranged pin reaching to the inside of the cap.

The invention is explained in detail below with reference to the drawing. Figure 1 shows a section through the inventive Device (1). Figure 2 shows a particularly useful one Design of the closure piece. In the drawing:

1 outer wall of the cap

2 wall of the interior of the closure cap

3 Hood of the sealing cap

k Concentric cone in the hood

5 Interior of the cap

6 Space between the outer wall and the interior wall

7 ring groove in the wall of the interior

8 Closure piece to close the interior

9 Pin of the locking piece

10 Recess in the pin of the breech block

11 Plate of the locking piece

12 containers

13 Edge of the container opening

The closure cap consists of two parts, the actual closure cap and the closure piece (8). The real one Closure cap is double-walled - the outer wall (1) encompasses the edge of the container opening (13) from the outside, while the wall of the interior (2) from the inside to the

7523561 26.0178

• 1 I ■ ·

Ma 223

The edge of the container opening (13). When the closure cap is placed on the container, the edge of the container opening slides into the space (6) between the outer and inner walls of the closure cap. The top of the cap forms a hood (3) that can be easily pushed inwards due to the elasticity of the material. On the inside of the hood there is a concentric cone (4) which engages in the corresponding recess in the pin of the locking piece (10). On the inside of the lower edge of the inner wall (2) there is an annular groove (7) _f into which the plate (11) of the closure piece engages.

The closure piece (8) consists of a plate (11) and one concentrically arranged pin (9). The pin carries the recess (10) already mentioned.

The interior of the closure cap (5) is charged with the substance to be dosed in the amount required for the reaction and closed with the closure piece (8) in such a way that that the pin (9) touches the hood (3) of the cap. In this way it is possible by pressing on the out elastic material formed cap to push the cap from the outside and thereby the contents of the interior of the To empty the cap closure (5) into a vessel closed with the closure cap. This is the one for the lock of the interior provided plate (11) to be pressed into an annular groove (7) of the interior, after which the plate is therein clicks into place. For easier fitting of the sealing plate into the The central pin (9) attached to the inside of the closure, as shown in FIG. 2, can also have an annular groove

7523561 01/26/78

• t ·

• ■ ·

be continued on the outside, so that the plate ■ can be guided into the locked position with the pin attached on the outside. The closure cap can be designed as a plug-in or very dust closure. The material used for the closure cap, including its interior, is an elastomeric plastic, for example soft polyvinyl chloride, preferably with 60-90 ° C. Shore, or a thermoplastic polyurethane elastomer with comparable hardness properties, which is sold, for example, under the protected trademark Desmopan® (Bayer AG, Leverkusen ) is available. The closure piece (8) with the central pin located on it is expediently made of non-elastic plastic, for example foIystyrene. The use of a material with a specific gravity> 1 is particularly advantageous at this point, because this sinks under the aqueous medium usually located in the reaction vessel and thereby facilitates mixing with the contents of the closure cap. Such materials are, for example, polycarbonates or polyvinyl chloride. In order to give the locking piece a specific weight> 1, a metal part can also be worked into it, for example into the pin (9). If iron or another magnetic material is used as the metal, the closure piece can serve as a magnetic rod after it has been introduced into the container (11). The size of the closure cap depends on the required reaction vessel and the interior space in particular on the required amount of the substance to be dosed. The one to be closed with the device according to the invention. The container only needs to be matched to the closure cap in the opening part. The shape and size of the container depends only on the reaction to be carried out in the container and its requirements.

7523561 01/26/78

The closure cap, the use of which as a metering device is also the subject of the invention, is in particular used for reactions that take place in several successive phases:

During a certain time, a sample solution reacts with a reagent solution, after which a second reaction is initiated in a second phase by adding a further reagent, in which, for example, a reactant is to be removed from the reaction mixture by complex formation, precipitation or adsorption. Radioimmunological and radiometric determinations of hormones and other components which are active in trace concentrations in the blood in solutions generally require such two-stage reactions. In determining the thyroxine content of the blood according to Murphy, B, EP, Pattee, CJ., "Determination of Thyroxine Utilizing the Property of Protein-Binding", J.Clin. Endocrine. Metob. 2A, 187 (1964), a thyroxine-containing extract of a sample of the blood serum was incubated in a first stage with a reagent containing thyroxine-binding globulin and radioactive thyroxine. Then a certain amount of an ion exchange resin is to be added to the reagent mixture, the batch is to be mixed and this mixture is then to be left to stand for a certain time. After the ion exchange resin has been separated off by sedimentation, the radioactivity of the solution or an aliquot is measured.

With the closure cap presented according to the invention, the following arrangement, for example, can be provided:

20-80 mg of a spherical ion exchange resin with a diameter of approx. 0.2-0.5 mm are weighed into the inner space of the cap and the cap is sealed in a liquid-tight manner as described. In a reagent tube, which is also useful

7523561 01/26/78

Ma 225 - 6 -

Made of plastic, about 3 ml of the will be required for the First incubation filled in the required reagent solution and sealed the tube with the cap. If necessary the cap is removed, the sample solution (0.3ml) added to the reagent solution and the reaction mixture with the closure cap according to the invention closed. The contents of the tube are then mixed for a while and incubated. After the incubation time has elapsed, pressure is applied to the domed hood of the closure cap over the pin The sealing plate is pushed out of its tight fit, after which the ion exchanger falls into the reaction solution. After The mixing time provided for the ion exchanger reaction is allowed to sediment the ion exchanger and is removed an aliquot of the supernatant solution for measuring the radioactivity.

The well-known radio-immunological ones run in a similar way Method for the quantitative determination of antigens (e.g. Houncne, Enzymes, drugs, etc.), which can be found in traces in body fluids must be proven. In the first stage, the sample solution is .with a reagent solution incubated in the next to the radioactively labeled Antigen to be determined, the specific antibody is contained in a defined concentration. The specific one Antibody is previously prepared by immunization according to known regulations by laboratory animals with highly purified antigen. Before measuring the radioactivity is from the reaction mixture a To remove reactants by precipitation, complex formation or adsorption. This is done in a second stage through dosed. "Addition of liquid or solid precipitants (e.g. ethanol, Propanol, ammonium sulfate etc.), complexing agents (antibodies in

7523561 01/26/78

Solution or immobilized on powdery carriers) or adsorbents (Ion exchangers, activated carbon, cellulose, etc.).

The closure cap according to the invention can be used as a metering device, for example, in the following way:

The one for felling. Complex formation or adsorption optimal amount of the liquid or solid reagent? is in the interior (5) -

_ measured or weighed and sealed as described. The test tubes serving as reaction vessels are made from radioactively labeled with the optimally adjusted reagent solution Antigen and specific antibody filled in a suitable volume and the prepared closures put on.

The metering of the reagent solution and the reagents of the second stage can advantageously be carried out with automatable metering devices and the implementation of serial examinations can be carried out in a very precise and reliable manner by semi-skilled personnel Instead of labeling with radionuclides, enzyme-labeled labels can also be used Antigens are used, the measurement finally being carried out photometrically.

If necessary, the cap <is removed, the sample solution added in a suitable dilution and, after thorough mixing, the reaction mixture is incubated for a few hours to days. To the The reaction products are separated in the second stage - without opening the tubes - through the closures in the caps Finger pressure on the hood of the caps is opened and the reagent for precipitation, complex formation or adsorption is added. After again The solid is allowed to settle in the reaction tube (if necessary with the aid of centrifugation) and measurements are taken the radioactivity of an aliquot of the supernatant.

7523561 01/26/78

• ■ " ·. ···;; Ma 225

Another example of the use of the test tubes according to the invention is the passive hemagglutination inhibition test, with which low concentrations of specific antibodies (virus, beasts,

Auto-antibodies etc.) can be detected and identified. In this case, the same amounts of the specific antigen are added as a so-called inhibitor to the dilution series of the serum to be examined and, after thorough mixing, the batches are incubated for about an hour. Erythrocytes sensitized with the same antigen (inhibitor) are then added and the reaction read off. If specific antibodies are contained, hemagglutination will occur in some of the tubes in the series of dilutions. The added amount of the inhibitor and the dilution of the serum in which the inhibition of ^{Häinagglutination:} visible uses, give information about the content of the specific antibody.

For these tests, the closure cap according to the invention can be used together with an iteaktionsröhr.chen meaningfully come. The inhibitor is optimally dosed into the The reaction tube is filled with the sensitized erythrocytes in the cap. Both reagents will due to better shelf life it is advisable to use lyophil

stored dry and sealed. For use, the cap is lifted and the lyophilized inhibitor is in the to be examined Serum dilution taken up and the incubation mixture mixed well by swirling the tube. After about one The erythrocytes are sensitized by pressure for one hour at RT added to the cap of the closure, the tube swiveled once for thorough mixing and the result after about one minute. The possibility /

to dose the two necessary reagents safely, quickly and precisely using suitable apparatus and none during use demanding precautions such as pipetting or other calibrations necessary to have.

7523561 01/26/78

Ma 225 - 9 -

For example, the determination of cholesterol and iron determination with dehydration should be mentioned for the usability of the tube closure for clinical-chemical reactions. In the determination of cholesterol by Liebermann-Burchard and acetic acid (7 mol / l) are filled into the container 2.5 ml of a mixture of acetic anhydride (6.5 mol / l) and in the closure cap ml 0.5 concen- ¹ - e sulfuric acid. To ensure chemical resistance to concentrated sulfuric acid, all parts of the container and the cap must be made of acid-resistant plastic, such as polyolefins. For use, the cap is lifted off, 0.1 ml of sample, standard or distilled water is added to the reagent mixture in the lower part of the container, the cap is replaced and the sulfuric acid is added by pressing the hood of the cap. After thorough mixing, the determination is carried out according to the usual procedure.

The determination of iron also serves as a further example of the application Deproteinization:. . ·

In the lower part of the additional filter you can find _ as a template. l ml a mixture of bathophenanthroline sulfonic acid disodium salt (0.68 mol / l), sodium phosphate (400 m mol / l), pH 5.5 and 300 mg Sodium acetate. The VeraAüiißkappe-5ng contains sodium ascorbate as a reducing agent. For use, the reducing agent is added to the reagent mixture by pressing the hood of the cap Cap removed and 2 ml of a deproteinized test person's serum, a standard solution or distilled water as a blank sample added. After thorough mixing of the reaction mixture, the measurement is carried out according to the known method.

7523561 01/26/78

Claims (3)

slogans. . 1. Closure cap that allows the storage and delivery of a allows dosed amount of a solid or ^ liquid substance in a vessel, characterized by a closable Interior (5), on the top of which a hood extends elastic material (3) with a concentric cone (4) and a closure piece (8), consisting of a plate (11) and a concentric pin (9), which is with a recess (10) at the end of the pin in the concentric cone (4) and with the outer edge of the plate (11) in a Ring groove (7) fits into the inner wall of the closure cap (2). 2. Use of reagents. 3. Use of the Vorpicntung according to claim 1 and 2 for storage and Abr * fbe of a metered amount of ion exchanger tinr rrrnimmi "iCnt-i 7523561 01/26/78