DD233491A1 - APPARATUS FOR PACKAGING SAEULES FOR FLUID CHROMATOGRAPHY - Google Patents

Abstract

The invention relates to a device for packing columns for liquid chromatography. The aim of the invention is to provide a technically simple device, can be produced reproducibly with the liquid chromatographic separation columns high Trennvermoegens. The task is to make the packing process with the help of a device so that the particles are exposed to minimal mechanical stress and still a high packing quality of Saeule is achieved. The task is solved by a swirling chamber in which a slurry stream impinges on a solvent stream.

Description

The device according to the invention consists of two stainless steel parts which can be screwed together to form a swirling chamber, the swirling chamber 3 and the swirling chamber cover 1. The columns to be filled can be connected to the swirling chamber via a column connection sleeve 5 provided with a matching thread. The sealing between the individual parts takes place by means of sealing disks made of PTFE composite material 2 and 4. The swirling chamber cover contains two holes arranged at right angles to one another, to which steel capillaries for supplying the solvent streams can be connected via corresponding cutting ring fittings. A possible dimensioning of the Verwirbelungskammer is shown in Fig. 1 as an example. The slurry medium is a solvent or a solvent mixture, which causes by its polarity, both a good wetting of the particles and their mutual repulsion.

Subsequently, a destruction of still existing or re-formed aggregates is achieved by a 5- to 20-minute treatment of the slurry in the ultrasonic bath. The thus prepared slurry is then added as quickly as possible in the slurry vessel.

At the second, fed into the swirling head liquid flow alone is the demand to make that it must be completely miscible with the slurry medium. By suitable choice of the swirling medium certain requirements of the packing materials (susceptibility to hydrolysis, wettability) can be taken into account as well as filling speed and filling pressure can be varied within wide limits.

The requirement of the slurry and the Verwirbelungsstromes via two separate pumping systems, whereby the setting of optimal packing conditions is easily possible.

In the swirling head, the supply lines of the two flowing media open such that a good turbulence and spatial homogenization of the suspension is achieved. In this case, the mutual position of the Zuführungskapillaren can be varied, and also replaced, and by incorporating further, the turbulence supporting parts (eg baffles) better mixing can be achieved. As low proves the lateral feed of the slurry, the connecting capillary leads to the middle of the swirling chamber.

As a result of this turbulence immediately above the layer to be packed, the slurry is permanently homogenized and already formed, loose aggregates are destroyed. The mechanical stress is so low that the packing particles do not break and no abrasion as in stirring occurs.

Advantageously, the actual separation column! when packing a 25 mm long guard column upstream, which connects directly in the lower part of the Verwirbelungskammergrundkörpers 3. This causes a whirling up of already packed layers

prevented. , '

Optimal column packing conditions can be achieved by choosing appropriate liquid media and independently variable streams. Suitable liquid media for use in the device according to the invention are, for. B. a 3: 1 mixture of carbon tetrachloride and dioxane as Slurrymedium and n-heptane as a pumping liquid or isopropanol as Slurrymedium and methanol as a pumping liquid for chemically modified silica gel of particle size

The separation columns for liquid chromatography packed with the device according to the invention are characterized by reproducibly good separation capacity. The packing procedure can be varied within wide limits and thus adapted to the respective packing material. By means of the device according to the invention, in particular packing materials that are not very resilient mechanically can be gently introduced into the separation column.

embodiment

2.2 g formerly modified silica gel (RP-18.10μπη) is suspended in a mixture of 10 ml of dioxane and 30 ml of tetra and homogenized 5 'in an ultrasonic bath. The finished slurry is placed in the slurry vessel through a steel pipe, i. D. 0.8 cm, is connected to the filling head according to the invention. The dimensions of the filling head can be seen as an embodiment of the drawing 1. The connected steel column has an inner diameter of 4.2 mm and a length of 250 mm. The feed takes place laterally with a flow of 4ml / min. The pumping fluid used is n-heptane, as well as the second, vertically injected turbulence flow with a flow of 20 ml / min.

During packing, the pressure increases continuously until the higher viscosity slurrymedium is purged with n-heptane. By increasing the swirling stream to 28 ml / min, the pressure achieved is kept constant and the packed column is left for 45 min. conditioned. After slow flow reduction, the column can be separated from the guard column and is ready for operation.

Claims (3)

Invention claim: 1. Chemical Methods By using liquid media with high density or high viscosity, the sedimentation of the particles is reduced. Additions of suitable chemicals (eg organic acids) should prevent the aggregation of the individual particles. 1. A device for packing columns for liquid chromatography, characterized in that a swirling chamber via a releasable connection (5) is placed on the head of a column to be packed for liquid chromatography, wherein the swirling chamber from the Verwirbelungskammerkörper (3) and the associated lid (1), the two connections, z. B. bores, which are preferably arranged perpendicular to each other, in which open capillary tubes, which serve to supply slurry or solvent. 2. Mechanical methods Almost complete spatial homogeneity of the suspension is achieved by stirring the suspension during the filling process. Ultrasonic treatment of the slurry causes destruction of already formed agglomerates and stabilization of the slurry. 2. Device according to item!, Characterized in that after screwing the Verwirbelungskammer is fed to a column to be packed via a column connection sleeve (5) through one of the capillaries slurry, while being fed via the other solvent, wherein the liquid streams collide in such a way that a Turbulence takes place. 3. Device according to item 1 and 2, characterized in that the feeding of slurry or solvent via separate pumping systems, which generate a pressure of 1.0 to 80 MPa. 4. Device according to item 1 to 3, characterized in that the supplied slurry or the solvent meet baffles. 5. The device according to item 1 to 3, characterized in that the slurry is fed laterally into the swirling chamber, wherein the connecting capillary leads to the center of the swirling chamber. 6. Device according to item 1 to 5, characterized in that the connection of the device of the column to be packed takes place via a precolumn, which has a length of about 25 mm. 7. Device according to item 1 to 6, characterized in that seals are made by PTFE molding. For this 1 page drawings field of use The invention relates to a device for packing columns for liquid chromatography. Characteristic of the known technical solutions The efficiency of any liquid chromatographic separation is substantially determined by the quality of the packing of the separation column. The packing material used is predominantly silica gels, chemically modified silica gels, aluminum oxide or organic polymers of very different structure and functionality, the use of silica gel and chemically modified silica gel predominating. In order to achieve a maximum separation capacity of the chromatographic system, the filler material classified as closely as possible must be brought into the separation column as a homogeneous, defined and reproducible packing. There are a variety of described methods and apparatus for making high separation column packages. The aim of all variants is to homogenize and stabilize a suspension (slurry) prepared from the separating material with a suitable liquid medium in such a way that aggregation of the particles as well as sedimentation during the filling process is minimized. 3. Apparative possibilities Attempts have been made to achieve improved packing quality by suitable arrangement of the column to the slurry vessel; to call z. B. up and down filling techniques. All enumerated variants usually contain one or more disadvantages. The solvents of the same density as silica gel, mostly halogenated hydrocarbons, are highly toxic; High-viscosity solvents require an enormously high pumping pressure (or a long packing time with the disadvantages of sedimentation and aggregation) and additives to the slurry often change the characteristics of the packing material or are difficult to remove. The agitation of the slurry leads to strong mechanical stress on the particles, so that they can break or simply deteriorated by abrasion, the column characteristic. Ultrasonic treatment during the packaging process is disadvantageous because it does not restrict itself to the slurry vessel and prevents the closest possible packing of the particles in the column. Differences in column and slurry vessel arrangement did not bring significant improvement in package quality. Above-average rapid packing of the column (by pressure-constant filling techniques) causes an increasingly loose packing of the last introduced particles, moreover, due to the rapid layering, no densest possible packing is to be expected (orientation of the particles). , , , ; .-: · · · ... ^ -....-.-.- '. Object of the invention The aim of the invention is to provide a technically simple device, made with the liquid chromatographic separation columns of high separation capacity reproducible and with which the disadvantages of known solutions can be overcome. Explanation of the essence of the invention The invention has for its object to pack separation columns for liquid chromatography reproducible with high quality. The particles should be subjected to only minimal additional mechanical stress, so that their given size and structure are retained. The object is achieved in that a device is constructed such that in a fluidizing chamber at the top of the column, the pumped slurry with a second liquid stream, preferably consisting of solvent, is mixed. The swirling head is expediently adapted to the particular design principle of the separating column. However, DrinziDiell has the structure shown in Fig. 1.