DE1498671B2 - Column for very accelerated chromatographic processes - Google Patents

Description

The invention relates to a column for very accelerated chromatographic processes, consisting from a tube with a capillary outlet, in front of which a porous frit is arranged.

Chromatographic separation columns have become known (Zeitschrift für Tierphysiologie, Tiernahrung and Futtermittelkunde, Vol. 18, 1963, p. 151, 152) which at its lower end has a porous Have frit, which is followed by a capillary.

The transition that opens into the capillary under the frit should be so tight and so small have remaining harmful space, as the applied glass technology just allows.

In columns of this type, in which the insertion of the pattern, the opening and closing of the columns Assuming ordinary hand cuts, it is difficult to find an accurate and simple one Way to ensure adjustable position of the expansion seal of the columns and a free one with To allow liquid-filled space above the filling of the columns, as in the case of new, very accelerated and in particular fully automated processes is necessary.

The invention is based on the object of creating a column which is simple and interchangeable Parts built up and yet unrestricted for very accelerated and chromatographic processes suitable is.

According to the invention this object is achieved in that the tube with its lower end directly or with the interposition of a transition piece placed on the face on an elastic sleeve is, which is inserted into a sleeve having the capillary outlet, in which the frit and an underlying elastic disc are arranged, which has a capillary opening in the middle and is grooved on its upper side, and that the tube is secured against the sleeve by means of is pressed on a rod attachable bracket and adjusting means with adjustable pressure.

Further features of the invention can be found in subclaims 2 to 6.

As a result of the proposal according to the invention, a simple cylindrical tube can be used as the column column with the help of the elastic cuff and the capillary outlet Sleeve, as well as the bracket and adjusting means is tightly closed at its lower end. The locking the tube with the help of a separate sleeve also enables the interposition of transition pieces, so that tubes of different diameters are used together with the same sleeve can be. In that the contact pressure of the tube against the sleeve under mediation the cuff is adjustable, the contact pressure can be applied to both the process pressure and the The thinness of the tube used can be adjusted. The contact pressure is therefore not exactly necessary be large that a reliable seal is ensured without the tube in its longitudinal direction is excessively stressed.

An embodiment of the invention is described below with reference to the drawing. It shows

F i g. 1 is a side view of the column carrier,

F i g. 1 a a section through the chromatographic tube,

F i g. 1 bb a plan view of the upper bracket,

F i g. 1 cc a plan view of the locking bracket,

Fig. 1 b, lc, Id each different Ausfüh-Tungsformen of rings to be placed on the tube,

F i g. 2 shows a section of the column arrangement with a tube of smaller diameter in section,

F i g. 3 shows a section of the column arrangement with a tube of larger diameter in section,

F i g. 3a is a side view of a partially impermeable frit,

F i g. 3 b a washer in a view and as a top view,

F i g. 4 shows the side view of a carrier with several connections distributed over its length to 'a second carrier,

F i g. 5 a view of the temperature control jacket of the colonins and the chromatographic tube,

6 shows a cuff connection on an enlarged scale Snippet display.

The chromatographic tube 1 here is a complete one smooth z. B. glass tube, which is of straight end faces is limited, the wall thickness of which corresponds to the pressure used. The inner space of the Tube 1, which is intended for its chromatographic filling, is at the bottom through a disc 2 (frit) from porous mass z. B. made of sintered glass, porous polytetrafluoroethylene and other completed ·. The frit 2 is inserted into a sleeve 3 made of a porous mass, e.g. made of silicone rubber. In the Cuff 3 under the frit 2, a disk 4 is possibly also inserted, which has a small opening and on its upper side grooves or Has incisions and the like.

The cuff 4 with the inserted parts 2 and 3, which can be inserted tightly in it, is in the the cavity of a chuck 5 and this possibly inserted loosely, in 'one of the FIG. 1 a visible Art.

The chromatographic tube 1 pushes the cuff 4 in the downward direction into the chuck S, whereby a sufficiently perfect seal both of the tube 1, as well as that in the cuff 4 inserted parts 2.3 against the chuck 5 is achieved, this being centrically by a capillary Channel is pierced, in which a flexible outflow capillary 6, without any dead spaces, z. B. made of polytetrafluoroethylene and the like opens. The capillary 6 is best with a sealing ring 7 Sealed from silicone rubber, which is sealed by a ring8, e.g. made from stainless steel or polytetrafluoroethylene through a hollow screw 9, which has a knurled edge for a delicate Tightening the seal 7 is provided by hand, on the one hand, the necessary sealing of the capillary 6 and, on the other hand, adequate resistance to any withdrawal from the To reach the stuffing box, if not other precautions against unwanted pulling out are provided. So that the chuck 5 does not rotate when the screw 9 is tightened, it can with this Manipulation can be held by a transverse pin 10 or by a disk 11 shown in dashed lines,

The chromatographic tube 1 is surrounded on the outside with an ordinary temperature control jacket 13, the in the usual way by rubber stoppers 14 and 15 is sealed, which can advantageously have one or more grooves on their circumference, in order to achieve a good seal without excessive lateral pressure on the jacket 13. The supply line and drainage of the temperature control liquid can be carried out in the usual way through glass tubes be, which are either melted into the jacket 13 from the side or through tubes 16, which advantageously open at an angle into the space of the jacket 13, which on the one hand saves space and on the other hand, the circulation in the jacket 13 of the column is ensured. The chromatographic Tube 1 can be arranged eccentrically in jacket 13. The lower plug 15 can be directly on the Place tube 1, as on the left half of FIG. 1 a is shown, or on the chuck 5, according to right half of Fig. la. In the first case there is the advantage that the feed 5 from 'the column can be taken without dismantling the jacket 13, in the second case that the column up to its The end is tempered and that possibly the chromatographic tube 1 through a smaller one Diameter can be exchanged, as will be stated below, without exchanging the lower one Stopper 15 ', which in this case lies on the lining 5.

The possibility of using smaller diameter tubes with chromatographic tubes a minimum number of components that may be replaced is shown in FIG. 2 shown. The right half shows the possibility of using a centric, possibly metallic Ring 17, which is the narrower chromatographic tube 1 in the feed 5, which is intended for further columns is centered. The seal between the tube 1 and the ring 17 is e.g. B. by a rubber ring 18 carried out. The left half shows a variant in which the centering ring 17 'itself is made of elastic or plastic material, and optionally with a ring 19, e.g. stainless steel is underlaid, which is necessary in such cases when it comes to a tube 1 of significantly smaller diameter than that of the frit 2 goes. Of course, you can also use the narrower tube 1, parts 2, 3 and 4 are exchanged to match the reduced diameter correspond better if the upper plug 14 of the column jacket 13 has to be removed or fill the free circular ring with a sealing insert is.

In FIG. 2 shows the possibility of a further embodiment of a lower chuck 5, see above that this is used at the same time to feed further liquid, gas bubbles and the like into that from the column exiting eluate can serve, as is necessary in some newer processes. Connecting the corresponding capillary feeds is shown in FIG. 2 in the usual way with the aid of a screw connection shown (with nut connections of the capillaries not shown).

Fig. 3 shows the possibility of use of essential parts of the column also when replacing the actual chromatographic Tube 1 through a tube with a larger diameter than the original one. The process is essentially the same as when using reduced diameters according to FIG. 2, only that the fixed centering ring 17 "and the elastic ring 18" of the reduction to a larger one Diameter instead of a smaller one. The F i g. 3 shows an expedient, as uniform as possible Reduction of the diameter from the chromatographic tube 1 to the one used Frit 2. On the left side of the FIG. 3 shows a 2 "frit in a conical design, which for the better formation of the exit of the concentrated wave surfaces at the exit from the Tube 1 in the capillary outlet can be advantageous. When in the middle of the tube 1 the track and the hydraulic resistance which the exiting eluate has to overcome is smaller than on the circumference

5 6

are, a certain compensation in simple jaw 26 has, which has an enlarged bore

Way (except by a shaped frit) thereby it has 27 for the free passage of the rod 20 and

■ will be enough that even with a flat frit the with the fixed part with the help of the thin bridges 28

Lengthening of the orbit and the enlargement of the or 29 are related, which is a sufficiently small

Resistances for the particles, which are in the middle 5 rigidity for the necessary small movements

of the tube 1, is caused by the fact that the jaws 26 have above the tube 1 so that they

middle part of the frit 2 is made impermeable, essentially as the articulated connections of the jaws 26

z. B. function by gluing or sucking in an impenetrable with the fixed part of the bracket 24. In

casual material, as shown in FIG. 3a is shown. the F i g. 1 ■ are two possibilities of a suitable one

A similar ¹ purpose is shown in the execution of the technological implementation of the bridge;

of the washer 4 as from the two views the bridge 28 is created by cutting off the gsstri-

the F i g. 3 b can be seen. The central capillary chelts indicated corner of the bracket 24 or through

The opening here does not go through the entire thickness of the hole in the bracket 24 indicated by dashed lines

Washer 4, however, is a connection through some prior to making the incision 24 '. The cheek

Channels drilled through at an angle in the circular grooves or 15 26 has a toothed opening 44, which may be at the front

Incisions made near the perimeter. The in the plan of FIG. 1 displayed art

Eluate flowing through the center of the tube 1 must be cut through, into which the upper end of the

describe an elongated path, similar to the chromatographic tube 1 either directly or

which executes the liquid on the walls to better fall through rings 45 and 30, as from the

to get to the outlet opening. The sealed 20 Fig. 1 can be seen. The ring 30 is through moderate

or the cemented-up point in the middle of the frit 2 can bend around its diameter beforehand.

possibly wear a cemented body, from det that he the pressure of the jaw 26 on the ring 45,

z. B. conical shape according to Fi g. 3a, which transmits the same and the tube 1 and is centric in essence

if a simple universal joint is used to reduce the undesirable deformity and function,

tion of the concentrated wave surfaces of the 25 The ring 45 is mainly for better distribution

End of the tube 1 exiting eluates contribute to the punctiform pressures determined by which

can. the ring 30 acts on the parts below and this

A complement to the tube 1 is its holder or on the diameter perpendicular to that part Carrier which is advantageously designed in a manner which the pressures of the jaw 26 on the ring we like is shown in FIG. 1, which is not just one ge 30 ken, as in FIGS. Ib and 1c in two examples suitable type of attachment, but also to see a simple design of the joint the one used to seal the lower tube cap. The ring 30 can by choosing its height and The necessary pressure ensures, furthermore, that the material is comfortable so that it is emptied at the same time the column filling allows and also tig forms an elastic intermediate link that does not the possibility of advantageously absorbing the large changes in the pressure on the tube 1 upper lock and, if necessary, further secures, if they arise during operation - Parts and units ordered near the tube, e.g. as a result of unequal thermal expansion should be offers. Some parts of this trä- tere small differences in the lengths of the Gers can optionally also be used to intercept the carrier and the column, their temperature control serve two or more tubes. 4 ° can change by around 50 ° C and more.

The base of the support, as in Fig. 1, for an elastic element that also performs this function

Tube 1 is shown, is a round rod or a and also has the function of an elastic gel

another profile 20, on which the individual transverse bracket kes can meet in the lower end of the tube 1 is

for intercepting the tube 1 and possibly also the rubber seal 3 itself,

also other parts slidably pulled up and in 45 Another elastic pad, also out

suitable adjustable position are attached. Rubber, can between the ring 45 and the top

A lower bracket 21 has, for. B. the form can be inserted according to the end of the tube 1, whereby the same-

F i g. 1 with distanced recesses or tough times the distribution of the punctiform pressures that

nen 22, in which a step 23 of the sleeve 5 is caused by the ring 30 on the parts below it

can be let. So that this can be improved even more comfortably through Aus 5 °.

Pushing the tube 1 by moving it from the front Pressing the tube 1 onto the cuff 3

can happen, the deposit 22 is shallow and the and the lining 5 against the lower bracket 21 (for

Bracket 21 cut through, similar to this control, whether the tube 1 with sufficient accuracy

is the case with the upper bracket 24, as it is from the speed concurrently with the rod 20, which is through

Plan view of Fig. 1 a is visible. 55 a correct position of the bracket 21 and 24 on the

All brackets can be placed on the rod 20 in a uniform manner

rather be attached way, e.g. B. so that their openings screw together and tighten a fine

gen for the rod 20 and cut with a screw 31, which is used for the sensitive adjustment of the

Screw 25 are tightened. Seal pressure is determined, which is based on the

The upper bracket 24 (Fig. 1, 1 bb) has an ahn- 60 sealing collar 3 transmits,
Lohe function for the interception of the tube 1 like the mentioned possibility of a direct interweaving lower bracket 21, but in addition it is with a recommendation of the jaw 26 to the tube 1 without the ring-sensitive device for regulating the pressure 45, 30 calls a hard point-like effect of the equipped that acts on the tube 1. This will exert all the pressure on the tube 1; one must achieve by, for example, see Fig. 1, that the bracket 24 65 necessarily count on the fact that this is divided into a single point on the circumference of the upper end by an incision 24 ', apart from that on the rod 20 firmly clamped (with due consideration being given to the fact that the jaw 26 ren part is only slightly movable angularly to that which acts like a joint

Bridge 28 and 29 slopes). If the tube 1 short and voltage or special holding devices) that a

is strong, the eccentric point pressure from the upper bends of the ring 30 must be relied on.

Jaw 26 will not act deleteriously on them. With long borrowed on the material of the jaw 26 is supported and not

and slender tubes, however, it is beneficial to collapse into their incision. When removing the

Measures to be taken so that their buckling strength, on 5 upper fastener 32 ', is not cut through

which they are burdened is not reduced in size. Except for the jaw 26, the closure 32 'is removed from the tube 1.

these listed constructive measures to be taken out. If after loosening the tube 1

ensure a centricity of the acting forces, from the jaw 26 the upper part of the chuck S from

it is advantageous that in the case of long tubes at the protruding lower end of the tube 1

Selecting the material to their straightness and genü- io is excluded, can offer the insertion of the

Attention must be paid to the wall thickness, whereby there is the filling of the tube 1 in the lower bracket 21

it is necessary that it be protected from internal stresses. Tube 1 by the action of the liquid flowing over

are free. Not only is this convenient from the standpoint of filling the top cap 32 '

security for the overprints applied and which and are gradually squeezed out. The filling

Buckling is important, but also possibly occurs here through the lower part of the tube 1 and 15

from the standpoint of security against expansion by opening the bracket 29 into a prepared one

print the cuff of an upper retractable receptacle.

Closure 32 'if this is used in the tube 1, so if the length of the tube 1 is greater, none

will be. too large bends of the rod 20 by the

When using this closure 32 'it is ao flow to seal the tube 1 properly necessary that it is freely pulled out of the tube 1, necessary forces occur, as something exaggerated gen can be. The rings 45, 30 are therefore shown in FIG. 4 without the need for and also the jaw 26 centric openings, which is the profile of the rod 20 and thus the size are larger than the inner diameter of the tube 1. to enlarge the bracket 21,24,33, one can through The closure 32 ', which is shown in dashed lines in FIG. 1, achieves the measure shown in FIG is placed, after being pushed into the rod 20, there is too much deflection Tube 1 to be fixed, namely in a new connections 38 to be eliminated, which at several Position with the help of another locking bracket 33, put the forces on a stronger carrier 39 which is transferred in the side elevation in Fig. 1 and in the plan in, e.g. of Fig. 1 cc can be seen. The bracket 33 is screwed onto the 30. The carrier 39 itself can be rod 20 be fastened in the same way as the previous quem on the frame of the device. Bracket 21, 24 attached, but has the option at the front. Fig. 5 shows schemati'sch how the temperature control mutual small movements, in the jacket 13 of which the tube 1 is long and slender after loosening a hand screw 34 between stiffening the chromatographic tube 1 used the jaws can become the protruding part of the closure 35 when in the space between the at-32 ' or another type of closure inserted into the tubes 1, 13 one or more inserts 40 are inserted can. Once the correct position has been determined, it can be pushed, reducing the buckling strength of the of the closure 32 'against the tube filling, tube 1 is considerably enlarged. The deposits 40 then the closure 32 'in this position by the connection must be carried out and attached so that the tightening the hand screw 34 fixed. The flow of the compensation fluid is possible in both. The shape shown allows for very simple interception of the Chen generation possibilities to reach the tube 1 in the brackets 21, 24, 33 described unnecessary mechanical properties for which is necessary or unsuitable, the inclusion of the Formation of a bridge (which in turn has a loading sleeve 3 between the lower end of the chroma path Articulated connection of the movable and photographic tube 1 and the opposite one most baking represents) through the incision 35 and surface of a Absohlußteils 41 by a screwing device pre-drilled opening 37, which are carried out at the same time by exercise, being part of the Veroben Access to the regulating screw 31 and screw on the tube 1 is cemented. forms the bracket 24 (Fig. 1 cc). 6 shows an example from the series

The toothed opening 28 of the bracket 24 must be possible in front of 50 ways of performing this type of one not be cut through, as in the closing of the cuff 3. The lining 5 in the pre-Fig. 1 bb is shown, if not on the advantage going cases is here in essence on three parts the cut through is reflected, d. That is, that is then divided: a closing part 41 contains a hollow one the tube 1 also with the inserted locking screw 42, which the closing part 41 against the Man-32 ' from the holder in the brackets 21, 24 slightly 55 schette3 (and the tube 1) and also against the can be pulled out. Through the non-through pipe nut 43, which is cemented onto the tube 1, however, there is the advantage that no pressure is cut. The other names have the same Safeguard must be made (due to the operating meaning as in the previous cases.

1 sheet of drawings

Claims (6)

Patent claims: 1. Column for very accelerated chromatographic processes, consisting of one tube with a capillary outlet, in front of which a porous frit is arranged, characterized in that that the tube (1) with its lower end directly or interposed a transition piece (17) is placed on the face of an elastic sleeve (3), which is inserted into a sleeve (5) having the capillary outlet, in which the frit (2) and an underlying elastic disc (4) are arranged which has a capillary in the middle Has opening and is grooved on its upper side, and that the tube (1) against the cuff (4) with the aid of brackets (21, 24) which can be fastened to a rod (20) and adjusting means (31, 26) is pressed with adjustable pressure. 2. Column according to claim 1, characterized in that a sleeve (5) holding the lower Bracket (21) and an upper bracket (24) holding the tube (1) at its upper end are provided are, which consists of two connected by an articulated connection (28, 29), arranged one above the other Parts consists of which the upper part can be fastened to the rod (20) and the lower part is designed as the tube (1) holding jaw (26), and that the parts by an adjustable Screw (31) can be pushed apart. 3. Column according to claim 2, characterized in that the tube (1) in the jaw (26) is held by means of a pressure ring (30) supported tiltably on the jaw (26). 4. Column according to one of claims 1 to 3, characterized in that on the rod (20) a further bracket (33) can be fastened to which one can be pushed into the upper end of the tube (1) Closure plug (32) is held. 5. Column according to one of claims 2 to 4, characterized in that the rod (20) means their deflection exerted on them in the longitudinal ■ direction by the bracket (21, 24) Force preventing holding means (38) is attached to a carrier (39). 6. Column according to one of claims 1 to 5, characterized in that in the case of one The tube (1) surrounding the temperature control jacket (13) supports it radially on the temperature control jacket Intermediate rings (40) are provided which have a passage for the temperature control liquid.