• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Chromatographic sheet of layer for pressurized layer chromatographic apparatus, for the development of linear chromatogram, which is characterized by sealing the sorbent layer at the edges of the sheet of layer applied conventionally with normal or fine-grained sorbent layer, and the sorbent layer is removed in one or several zones near the place of solvent admission, or one or several baffle plates or wires are arranged behind the sample application place or places, and -if necessary- it is provided with conventionally formed concentrating zone on the part from the direction of the solvent admission. The developing solvent composite does not escape at the edges of the sheet of layer in case of overpressure, and it advances with straight front.
    公开号:SU1531866A3
    申请号:SU813315648
    申请日:1981-08-05
    公开日:1989-12-23
    发明作者:Тьихак Ерне；Минчович Эмиль；Тетеньи Петер；Калас Хуба；Надь Янош；Кнолл Йожеф；Золтан Шандор；Лак Иштван
    申请人:Лабор Мюсерипари Мювек (Инопредприятие)；
    IPC主号:
    专利说明:

    31
    the form of wires 6 (fig.) or plates 7 of synthetic film (fig. 4), or grooves 8 are located, the base of which is substrate 1 (fig. 2) One or more wires 6, plates 7 or grooves 8 may be located on the plate, offset relative to each other. The width of the grooves is 0.1–0.5 mm, the wire diameter is 0.05–1.0 mm. The maximum length of the grooves, wires or plates is equal to the length of the sorbent layer remaining after sealing the edges, but in the preferred embodiment - shorter by 1–20 mm
    In the zone 4 of the supply of the solvent can be located inactive zone 9 concentration, the length of which corresponds to the width of the layer of sorbent I (Fig. 3)
    In order to form a concentration zone, one more layer is applied to the sorbent layer, consisting, for example, of silica glass powder, synthetic powder or secondary cellulose acetate. Silica gel can be applied with high porosity and a wide range of pore sizes. The layer of sorbent can be sealed with two, three (Fig. 1-3) or four, (Fig. 4) sides. With one-dimensional .YM of occurrence, it is sufficient to seal the two edges of the layer, as well as the side opposite to the direction of propagation of the appearance front. In the case of two-dimensional development, it is advisable to seal the layer on all four sides. In the case of a two-dimensional linear appearance with an intermediate introduction of the solvent, it is sufficient to seal the two opposite edges of the plate. The width of the sealing layer may be 0.05-3 cm. The length of the layer is equal to the length of the chromatographic plate. Sealing of the sorbent layer is carried out by impregnating, glazing or sintering with porous glass. Paraffin, synthetic solutions or suspensions, soda glass (sodium silicate) can be used as a material for impregnation. The edges of ceramic plates can be coated with white tin and lead-lead glaze.
    Example 1.110 ml of an 85% aqueous solution of a relatively highly polymeric called homopolymer polyacrylamide is added to 32 g of silica gel powder with an A-8 µm particle size and an inner diameter of 60 A. After





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    35
    50
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    After mixing, the suspension was applied in a layer with a thickness of 0.25 mm onto a non-fat glass substrate cm, 1.5 mm thick. Layers dried at room temperature have high mechanical strength even after activation.
    The edge of the thus obtained and activated plate is impregnated across the width of ID mm. by immersing the three sides of the plate in industrial paraffin, melted at 30 ° C.
    To direct the solvent, a steel wire with a diameter of 0.2 mm is placed in front of the insertion point (Fig. 1). Using methylene chloride as a solvent, natural dyes (zinc yellow pigment, Sudan G and indophenol) are separated; the pressure of the pad in the ultra-micron chamber is 1.0 IPa, the development time is 10 min, the distance is 15 cm.
    Example 2. The plate was made in the same way as in example 1, but instead of 32 g of silica gel powder, 30 g of neutral alumina with a grain size of 15–20 µm, a layer thickness of 0.3 mm, are used.
    Example 3. 100 ml of a 1.8% aqueous solution of acrylamide polymer and an acryloxy acid anionic mixture with a low degree of polymerization add silica gel with a granule size of 4-5 µm and an inner diameter of 60 A to the powder. After thoroughly mixing, the suspension is applied in a layer 0 3 mm per poly terephthalate foil with a thickness of 0.4 mm and dimensions of 20 "40 cm. The layers are dried at 75 ° C and have sufficient strength even after activation. Immediately after application, prior to the aforementioned drying, for the purpose of subsequent control, a Foil strip 2 mm wide, 0.3 mm thick, and 185 mm long, is placed 15 mm from the average impregnated edge of the plate and at an equal distance from two side impregnated edges (Fig. I). Such a strip sticks to the layer during the drying process. The edges (from three sides) of the thus obtained dried plates with layers supplied with control strips (from foil) are impregnated with immersion in a 1, 5% aqueous solution of highly polymerized non
    ionogenic polyacrylate homopolymer 5 mm wide and dried at room temperature. Discrete glycosides are effectively separated on the obtained plate in a linear ultramicron pressure chamber under the influence of a prostrate of Yautanon-2 under a pressure of 1.0 MPa, at a distance of 35 cm in 18.5 minutes,
    Example 4. The manufacture of the plate was carried out in the same manner as in Example 2, but to control the solvent in the layer, two grooves with a width of 3 mm each were formed (Fig. 2).
    Example 5. 100 ml of a 2% aqueous solution of polyvinyl acetate is added to 26 g of silica gel powder with a granule size of 8-10 µm and an inner diameter of 60 A. At the same time, 50 ml of a 2% aqueous solution of polyvinyl acetate is added to B g of silica with a grain size of 10-20 microns. Both systems are homogenized in separate electric homogenizers for 1 minute, after which the resulting two suspensions are spread in a solid manner using two trays, respectively, separated in length, and applied to aluminum foil 0.2 mm thick and see dimensions. In this way, a two-zone is obtained. a sorbent layer with a thickness of 0.25 mm, in which the width of the inactive zone (corresponding to the distance between the trays) is 40 mm.
    Before drying the sorbent layer (immediately after applying the suspension), a plate made of polyterephthalate 0.3 mm thick, 1 mm wide and 160 mm long, is placed 15 mm from the average fillet edge of the plate and at an equal distance before the point of the intended introduction of the solvent. from two other parallel edges soaked in order to control the flow of solvent.
    Then the layer is proscupt, and in some cases it is activated.
    . The impregnation of the edges of the plate is performed in the same way as in Example 2.
    On the layer thus formed, equipped with a concentration, the components (sesquiterpenes 11) of samples of volatile oils obtained by steam distillation of Matricaria Chamonix L. Pa flowers are effectively separated. Pa: the separation is carried out in
    866
    , a linear pressure chamber with benzene as a solvent at a pressure of 0.7 MPa for 12 minutes at a distance of 15 cm, the bulk velocity of the solvent is 20 ml / h.
    Example 6. The production of the plates was carried out in the same way as in example 4, but instead of 8 g of silica, 7 g of cellite in a powder with a granule size of 10-20 µm was used.
    Example 7. 36 g of magnesium silicate powder with a grain size of 6-10 µm and PO g of an aqueous solution of sodium silicate with a fortress of 6 Baume are homogenized in an EL of a 2-grinder and applied in a usual manner onto a single glass plate with a thickness of 1.5 N1M. These plates are placed in a chamber with a relative humidity of 75% for 2, .5 h, then removed and sieved at room temperature. So get a layer with sufficient resistance. Kra obtained plates
    5 is impregnated in the same manner as in Example I. They can be used as effectively for the separation of coloring matter.
    Example 8. Plasma manufacturing (3 tons is carried out as in Example 3, with the difference that two opposite long edges of the plate are impregnated before the sorbent layer is dried by immersion in a 1.5% aqueous solution of highly polymerized non-ionic polyacrylamide homopolymer. At the same time, a 1 mm-wide groove is made in the center of the layer at the point of introduction of the solvent for the next control of the distribution of the solvent in the case of a two-dimensional display. Then the layer is dried and used.
    Example 9. The manufacture of plastics and tins was carried out as in Example 7, but the layer was prepared for two-dimensional development by impregnating all its four sides. The solvent spreads as shown in
    0 fig. four.
    Sealing the edges of the plate eliminates solvent leakage when separating mixtures in thin-layer chambers under excessive pressure. The arrangement of the grooves, wires or plates of synthetic film on the plate ensures the straightness of the front of movement of the solvent. Concentration zone enhancement contributes to good
    five
    concentrations of pasAenHCMbix samples before separation.
    权利要求:
    Claims (2)
    [1]
    1. Chromatographic plate for a pressure-rich thin layer chromatography device containing a substrate with a layer of fine-grained
    sorbent and sample and solvent delivery zones,
    distinguish

    so that at least two edges of the sorbent layer are sealed, and between the sample and solution supply areas
    The solvent has at least one groove, the base of which is the substrate, and partitions installed in the vnde wires or plates are installed, while in the solvent supply zone there is an inactive concentration zone, the length of which corresponds to the width of the sorbent layer.
    [2]
    2. Plate pop. 1, characterized in that the sorbent layer is sealed by impregnation, glazing or sintering with porous glass.
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    Compiled by V.Tolstykh Editor N.Lazarenko Tekhred L.Oliynyk
    Fi.Z
    Proofreader V.Kabatsiy
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    同族专利:
    公开号 | 公开日
    US4591524A|1986-05-27|
    EP0042393B1|1985-10-30|
    EP0042393A4|1982-04-22|
    HU184065B|1984-06-28|
    WO1981001746A1|1981-06-25|
    JPS57500083A|1982-01-14|
    DE3071215D1|1985-12-05|
    EP0042393A1|1981-12-30|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    CH364130A|1961-05-10|1962-08-31|Brenner Max|Process for performing thin-layer chromatography and apparatus for performing the process|
    US3482943A|1966-02-14|1969-12-09|Miles Lab|Reagent deposition device|
    GB1183836A|1967-09-04|1970-03-11|May & Baker Ltd|Improvements relating to Thin Layer Chromatography.|
    US3522792A|1967-11-14|1970-08-04|Us Agriculture|Device for applying a coating of varying thickness|
    US3714035A|1971-05-19|1973-01-30|D Jones|Method and apparatus for thin layer chromatography|
    JPS5216400B2|1971-12-17|1977-05-09|
    US3878100A|1973-02-01|1975-04-15|Marine Colloids Inc|Separation medium|
    US4065384A|1976-10-26|1977-12-27|University Of Illinois Foundation|Graft thin layer chromatography|
    SU752165A1|1977-07-28|1980-07-30|Институт Нефтехимического Синтеза Им. А.В.Топчиева Ан Ссср|Thin-layer chromatographic plate|
    US4126554A|1977-09-02|1978-11-21|Analtech, Inc.|Selectively marked thin-layer chromatographic plate|HU189133B|1982-04-28|1986-06-30|Labor Mueszeripari Muevek,Hu|Special layer plate and/or layer plate system for overpressure multi-layer chromatography|
    US4757004A|1984-03-16|1988-07-12|SyntexInc.|Chromatographic devices having modified edges|
    US4883688A|1984-03-16|1989-11-28|SyntexInc.|Method for producing chromatographic devices having modified edges|
    EP0169951A1|1984-07-30|1986-02-05|Varex Corporation|System and apparatus for multi-dimensional real-time chromatography|
    US5116495A|1987-09-11|1992-05-26|Ottosensors Corporation|Capillary chromatography device|
    US6303029B1|1999-10-25|2001-10-16|Advanced Research And Technology|Arrangement and method for performing chromatography|
    FR2843198B1|2002-08-02|2004-10-15|Bionisis Sa|DEVICE FOR SEPARATING CONSTITUENTS OF SAMPLES BY PRESSURE LIQUID CHROMATOGRAHY|
    EP1648582A4|2003-06-19|2010-02-17|Univ Indiana Res & Tech Corp|Method and apparatus for performing planar electrochromatography at elevated pressure|
    US8506802B1|2010-01-25|2013-08-13|Gaston De Los Reyes|Stackable planar adsorptive devices|
    CN102680638B|2011-03-15|2014-04-23|上海高佳仪器科技有限公司|Manufacturing method of overpressured thin-layer chromatography prefabricated plate|
    CN103566912A|2013-11-09|2014-02-12|四川师范大学|Liquid chromatographic stationary phase filler and preparation and application thereof|
    DE102017118530A1|2017-08-14|2019-02-14|QC1 GmbH|Plate for thin-layer chromatography|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    HUCI001995|HU184065B|1979-12-06|1979-12-06|Cromatographic layer sheet for a pressurized layer chromatographic equipment|
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