DE7019684U - MICRO SEPARATING COLUMN FOR LIQUID CHROMATOGRAPHY. - Google Patents

Description

G 10 424 G-bm

Mr. E. SCHUPPE and Dr. med. Kurt-Wilhelm STAHL, 3 Hannover, Schiffhornfeld 21

Micro separation column for liquid chromatography

The invention relates to a thermostattable micro-separation coil for liquid chromatography and especially for high pressure liquid chromatography.

So far known micro-separation columns for this purpose have the disadvantage that they are relatively cumbersome are to be handled and that they are of the desired size for each individual i'all ir manufacture nut. More!, ". Enteile consist of that the eluent to be examined can also come into contact with parts that are released from the elution » medium may be attacked.

The object of the invention is to avoid these disadvantages and a micro-separation column for jLiquid chromatography to create the no point is attacked by the elution agent

and so easy to put together and take apart is that separating columns of the desired length can be made from a few components.

To solve the problem posed, according to the invention suggested that the KSsro should be concentric on the outside Glass capillary held in an outer transparent cover and Arischlußteile for supply and discharge ueo zu investigating eluent and one to. Thermostat 'i' having serving fluid, which are easily detachably connected to one another. Such a Kikrot separation column can be disassembled into its individual parts in a few simple steps, with the additional advantage shows that the glass capillary including those surrounding it Sheath can be set down to the desired length in each case before the contouring, without the connecting pieces etc. would have to be changed.

According to the practical embodiment of the invention, the microtrennsä ^ le has two head pieces, which are sealingly attached to both ends of the transparent cover detachably and which, also detachably, accommodate holders for the glass capillary and connecting pieces for the liquid to be examined. The head pieces preferably have through channels for the fluid used for thermostatting. This fluid can thus flow through the outer shell and surrounds the capillary concentrically housed in the same.

According to a further feature of the invention, there are all parts with which the fluid to be examined (Eluent) comes into contact, from acid-resistant αϊ

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or made of material that cannot be attacked by the eluent. This means that the micro- "ΰX6iliiSaui.6 gaiiiilt

According to yet another Her lana 1 of the invention that carries upper head piece of the separation column an injection block, the injection opening with a pierceable septum is closed, which after removing the injection needle od. The like. Automatically closes ,, This septum is zv / corner secured against shifting in its holder. There is also a septum seal on the injection block releasably attached, which contains an adjustable connector, so that this closure to different long injection needles or the like

Further advantages and features of the invention emerge from the following description of the drawing, which represents a vertical longitudinal section through a micro-separation column designed according to the invention.

The micro-separation column has a connection piece 1 designed as a screw-in piece for an injection needle or the like. which is held adjustable by means of a lock nut 2 on a septum closure 3. The septum lock is fastened to an injection block 7 by means of a union nut 4-, with a septa occlusion between and injection block 7 one of an injection needle or the like. pierceable septum made of plastic like "Viton" with a thickness of about 2mm. This septum 5 is in mutually offset grooves 5a or other depressions in the top of the injection block 7 and the

i underside of septa holder 3 pressed when the I.

Union nut 4 is tightened. This avoids can be.

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The septum seal 3 is provided with an axial bore 3 a, which extends at its; Below the end 5b, widened in the shape of a funnel at an angle of about 30, so that the septum pierced with a Spxitz cannula or injection needle after the analysis sample has been taken can initially escape in the area of the puncture point when the cannula is withdrawn into the widened bore 3b and after the removal the cannula or injection needle immediately closes selbsttäti _L. In general the analysis TiTnV) O mi + T-7 i Ί f η oil) ior «omi 1 - + - mi — T. *" I \ r ~ nr \ ~] -> * f * Ä * F « a -τ \ τ · -ί + r7ovilrov.i "1 <- \

entered.

The axially adjustable connection piece 1 ensures in Connection cit of the lock nut 2 that the rlikrotrennsäule any cannula length of the HamaTtons syringe can be adapted so that the cannula tip is always immediately above the silica gel bed when the Hamilton's pritae has been introduced up to the shaft stop. This is very important because the goodness of the Ohromatogramtnes is decisively influenced by this. The Eiristichlzanal has exactly the same diameter as the injection cannula the Hamilton syringe.

In the injection block 7 is also a sealing cone made of V _? A steel used, to which a capillary 9 made of V ₂ A steel is connected via a brass L..tter β, which is used for the supply and inlet of elution

In the separation column according to the invention, the continuous supply of eluent into the column is as little as possible disturbed, whereby one extralumnal influences on the residence times of the individual substances to be analyzed Can reduce sample to a minimum.

The injection block 7 containing through bores is screwed into a head piece 21, with at its inner end of a plastic spacer 10 is provided. via sealing rings 11 and 12 the connection to the head piece 11 and to the upper end of an inserted glass capillary 16 is sealed. The glass capillary 15 extends through a transparent Material existing outer shell 15 to an opposite head piece 22 and is there with the help of a further spacer 18, which is also made of plastic, centered in a column end screw connection 17, which is screwed into the head piece 22 and consists of VpA- j steel.

The sleeve 15 is sealed via sealing rings 14 against the head pieces 21 and 22, which Kofpstücke in the outer inden the on each l; cases be trimmed desired length is screwed.

Connection terminals 13 and 13s are attached to the head pieces 21 and 22 attached, which are used for the supply and discharge of fluid intended for thermostatting. This Fluid flows through the outer shell 15 and thus around the glass capillary 16.

On the outer end of the column end screw connection 17, a sealing cone 20 made of Y ₉ A steel for connecting a further capillary (not shown) is fastened with the aid of a nut 19. This capillary can also consist of YpA steel.

All parts with which the eluxant comes into contact are preferably made of VpA steel> KeI Έ or glass. This guarantees that it can be used as universally as possible. The column can also be completely dismantled into its individual parts - septum holder, injection block, Liessing heads 21 and 22 with the hose nozzles, transparent casing, column end screw connection, glass column or - capillary and connection capillary - in just a few simple steps. It follows that by changing the length of the transparent envelope and the glass column with the same connecting pieces, a separation column of any length can be produced. Glass capillaries of the type used here are commercially available. The glassblower only has to grind the ends flat and also grind the lower end to the diameter of the spacer 18 consisting ^{of KeI i 1.} At the same time, a pilter plate can be inserted between the P-stopper and the glass capillary, which is intended to prevent loss of packing material from the column. The construction of the KeI F spacers guarantees automatic centering of the inlet and outlet openings during assembly.

The seal with Viton-O-rings shows at the entrance before. 25 atm using an eluent with a very low viscosity such as chloroform there is still no leak.

Expectations:

Claims (8)

, zansnrüche: 1.) Hikxotre "a: .. sävle for liquid chromatography, characterized in that they have a concentric in an outer through- visible envelope, 5) held glass capillary (Ib) and connecting pieces (7 or 13, 13a) for the separated Supply and discharge of the eluent to be examined and a water flow medium used for thermostating which are easily detachably connected to each other » 2.) Device according to claim 1, characterized in that it has two head pieces (21,22) which at both ends of the transparent cover (15) are sealingly and releasably attached and the, likewise detachable, brackets for the glass capillary (16) and connecting pieces for the r; u examining Absorb liquid " 3 ·) Device according to claim 2, characterized in that the head pieces (21, 22) have through channels (13,13a) for the fluid used for thermostating. 4.) Device according to claim 1, 2 or 3, characterized dadurcn, that all parts with which the fluid to be investigated (eluent) is in Contact comes, consist of material resistant to the eluent. 5.) Device according to claim 2, characterized in that the upper head piece (21) of the [separation column carries an injection block (7), the injection opening (3a, 3b) with a duichstechbaidn Septum (5) is closed, which closes automatically after removing the injection cannula. 6.) Device according to claim 5, characterized in that that a septum seal (3) is releasably placed on the injection block (7), the contains an adjustable connector (1). 7.) Device according to claim 5 or 6, characterized in that that the support on the injection block (7) and the septum seal (3) are flat for the injection septum (5) rotc against each other ver-j set recesses such as grooves v5a) are provided. 8.) Device according to claim 5, 6 or 7, characterized in that that the through hole (3a) of the septum seal (3) is at its inner end (3b) expanded like a funnel towards the septum (5).