US3752316A - Device for development in thin-layer chromatography - Google Patents

Device for development in thin-layer chromatography Download PDF

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US3752316A
US3752316A US00156766A US3752316DA US3752316A US 3752316 A US3752316 A US 3752316A US 00156766 A US00156766 A US 00156766A US 3752316D A US3752316D A US 3752316DA US 3752316 A US3752316 A US 3752316A
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solvent
chamber
development
support means
plate
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R Takeshita
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
    • G01N30/94—Development

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  • ABSTRACT A device for development in thin-layer chromatography comprising a solvent chamber, a support means, a plurality of horizontal bars and one or more plates for development.
  • the plate is suspended with a support means which can be rise or fall, and the lower end of said plate is soaked in solvent when it has become completely saturated.
  • This solvent chamber brings about a good result on the reproducible quality of R, values in thin-layer chromatography.
  • This invention relates to a solvent chamber for thinlayer chromatography in accordance with a method of absorption and partition analysis, especially to a device wherein compounds can be developed in the saturation of solvent vapor, and thereby precise analysis, the reproducible R, values were gotten, and the development was easily operated.
  • a plate for development is suspended with a devised support means which can be raised and lowered, and whenever the solvent in the chamber has become completely saturated, the lower edge of the plate is immersed into the solvent so that the reproducible R, values are always obtained.
  • this invention relates to a device for developing chromatoplates in thin-layer chromatography which is equipped with a hight-adjustable support means. They are made of such material as stainlesssteel or some kinds of plastics, which is proof aginst acids, alkalines, and organic solvents. To a lower part of the support means, some of horizontal bars are connected. Thus a plate for development is suspended from the bar so that its lower edge can be contacted with or separated from a solvent system in the chamber.
  • the plate can be lowered into a solvent without opening the cover of the chamber after saturation of solvent vapor, and then develpment can be started.
  • edge effect which is a phenomenone that solvent front is curved during development because of unsaturation of chamber, does not occure.
  • the development can be conducted with a relation that migration distance of the compound is proportional to that of the solvent. As the result, the R, value of any compound is obtained with excellent reproducibility.
  • the plates can be suspended with clips from some horizontal bars fixed up to the support means, a plurality of plates can be used for development, and raised or lowered smoothly.
  • FIG. 1 is the front view of the mode of an embodiment of this invention.
  • FIG. 2 is the cross sectional view of FIG. 1.
  • FIG. 3 is the cross sectional view of the second embodiment of this invention.
  • FIG. 4 is the drawing of the patterns wherein the distance of movement of a substance is shown by the longitudinal axis and the distance of permeation of solvent is shown by the transversal axis.
  • the solvent chamber 10 is made of glass, and in the shape of a somewhat deep box whose top is opened; its edge 11 is finished smooth so that its interior can be tightly shut with a cover 12.
  • the cover 12 is very tight and the support means 13 which also serves as a knob is fixed up approximately at the center of the cover.
  • Said support means 13 is composed of a guide pipe 14 fixed, a rod 15 inserted through the interior of the guide pipe 14 and a nut 17 screwed up to the screw part 16 of the rod 15.
  • a lower part of the guide pipe 14 is screwed up, and fixed with two ring nuts 18 and 19 from inside and outside of the cover 12, through a hole at the center of the cover.
  • the rod 15 is inserted through the interior of the guide pipe and can be rised and lowered byturning a ring 17.
  • a packing and other suitable sealing means may be put on the top of the guide pipe in order that solvent vapor in the interior of the solvent chamber 10 may not leak out of the space between the top of the guide pipe and a lower part of the ring 17.
  • a screw 26 which is screwed up to the screw hole of an arm 20, and the rod 15 is vertically equipped at a right angle to the arm 20.
  • the rod 15 is vertically equipped at a right angle to the arm 20.
  • At two sides of the arm 20 there are made a plurality of (four shown in the drawing) screw holes at intervals in the horizontal direction, and into each screw hole 22 there is fixed up a horizontal bar 21, from which the plate 24 of development is suspended by means of a clip 23.
  • the horizontal bars 21 are supported in parallel with one another.
  • the support means, arm and horizontal bars are made of a stainless steel or plastic materials that remain uneffected by several organic solvent, acids or alkali.
  • chromatoplates such as 5 X 10cm, 5 X 20cm, 20 X 20cm etc.
  • the embodiments shown in FIG. 1 and 2 respectively show a case in which each of two plates having the size of 20 X 20cm is suspended by means of each of two horizontal bars 21.
  • each of a required number of the plates having different sizes is suspended by means of each horizontal bar.
  • the rod 15 in the support means is replaced by an enormous rod or one enlarged by'connecting some joints 25a and 25b having a screw 36 respectively which is conjugated to the lower part of the rod 15 as shown in FIG. 3 so that the rod may have a required length.
  • each horizontal bar 21 is difficult to keep only by the arm 20, it is sufficient that a guide member (not shown) having the same shape as that of the support arm 20, is inserted into one end of each horizontal bar 21 and through the bar in order that the equilibration may be kept by regulating the distance between the horizontal bars 21.
  • the plate for development After a spot of a substance to be examined is applied to the plate for development 24, the plate is suspended from a horizontal bar 21 with the clip 23, and without immersing the plate into the solvent setinto the solvent chamber 10, in which amount of solvent 30 necessary for development has been put into the solvent chamber in advance. After the equilibration of the plate with solvent vaporis completely achieved in the chamber, the plate 24 for development is immersed into the solvent chamber by turning and adjusting the nut 17 of the support means and thus developed with the solvent 30. The rod of the support means 13 is made to rise, and the lower end of the plate 24 is kept from soaking in the solvent 30 in the solvent chamber. Namely, as the lower end of the plate 24 is distant from the solvent, in this condition there is no movement of any substance on the plate and development is not yet made.
  • the development curve of a compound is straight-line according to this invention, and especially at the initial stage of the development high precision can be obtained as compared with a conventional method.
  • Two thin and dotted lines shown in FIG. 4 show curves obtained when some compounds,
  • a device for deveopment in thin-layer chromatography comprising a solvent container, an air tight cover for said container, said container and cover defining an airtight chamber in which a quantity of liquid solvent is disposed, said chamber above said liquid solvent being saturated with said solvent, support means mounted on said cover and extending into said chamber, said support means suspending at least one developing plate within said solvent chamber, and actuating means operatively connected to said support means and actuable externally of said solvent chamber for raising and lowering said support means within said chamber, whereby said developing plate is subjected to the saturated solvent within said chamber above said quantity of liquid solvent before being lowered for immersion into said liquid solvent.
  • said support means comprising a guide tube mounted in said opening, a rod mounted in said guide tube, a rotary element disposed externally of said cover and operably with said rod to raise and lower the latter, and support elements within.
  • said enclosure mounted on said rod for holding said developing plate in a suspended disposition, whereby rotation of said externally mounted rotary element lowers said development plate.

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Abstract

A device for development in thin-layer chromatography comprising a solvent chamber, a support means, a plurality of horizontal bars and one or more plates for development. The plate is suspended with a support means which can be rise or fall, and the lower end of said plate is soaked in solvent when it has become completely saturated. This solvent chamber brings about a good result on the reproducible quality of Rf values in thin-layer chromatography.

Description

United States Patent 1191 Takeshita DEVICE FOR DEVELOPMENT IN THIN-LAYER CHROMATOGRAPHY [76] Inventor: Ryuzo Takeshita, No. 5-4-1 1, Koenzi Minami, Tokyo, Japan [22] Filed: June 25, 1971 [21] Appl. No.: 156,766
[52] US. Cl. 210/198 [51] Int. Cl. 801d 15/08 [58] Field of Search 210/31 C, 198 C [56] References Cited UNITED STATES PATENTS 1451 Aug. 14, 1973 Primary Examiner-John Adee Att0rneyDavid Toren et al.
[5 7] ABSTRACT A device for development in thin-layer chromatography comprising a solvent chamber, a support means, a plurality of horizontal bars and one or more plates for development. The plate is suspended with a support means which can be rise or fall, and the lower end of said plate is soaked in solvent when it has become completely saturated. This solvent chamber brings about a good result on the reproducible quality of R, values in thin-layer chromatography.
3,342,333 9/1967 Geiss et al.... 210/198 0 3,341,017 9/1967 Powell 210/198 c 5 Clams 4 Drawing Figures DEVICE FOR DEVELOPMENT IN THIN-LAYER CHROMATOGRAPHY This invention relates to a solvent chamber for thinlayer chromatography in accordance with a method of absorption and partition analysis, especially to a device wherein compounds can be developed in the saturation of solvent vapor, and thereby precise analysis, the reproducible R, values were gotten, and the development was easily operated.
As for conventional chromatography, after a compound to be examined is given to a plate to which adsorbent has been coated, the plate is placed aslant in a chamber by the wall of the chamber, in which solvent has been placed shallowly. If such an operation is conducted, the lower edge of the plate is immersed in the solvent and the plate is developed before the solvent vapor has saturated in the chamber. Therefore, any substance to be examined moves briskly before the adsorbent on the plate has fully been equilibrated with the solvent vapor. As the result of this development, time required for the saturation by a size of the chamber in which the compound has been developed, and the R, value obtained thereby is changeable.
In this invention, a plate for development is suspended with a devised support means which can be raised and lowered, and whenever the solvent in the chamber has become completely saturated, the lower edge of the plate is immersed into the solvent so that the reproducible R, values are always obtained.
Namely, this invention relates to a device for developing chromatoplates in thin-layer chromatography which is equipped with a hight-adjustable support means. They are made of such material as stainlesssteel or some kinds of plastics, which is proof aginst acids, alkalines, and organic solvents. To a lower part of the support means, some of horizontal bars are connected. Thus a plate for development is suspended from the bar so that its lower edge can be contacted with or separated from a solvent system in the chamber.
By using this devised means, the plate can be lowered into a solvent without opening the cover of the chamber after saturation of solvent vapor, and then develpment can be started. In the process of development, the so-called edge effect" which is a phenomenone that solvent front is curved during development because of unsaturation of chamber, does not occure. In addition, the development can be conducted with a relation that migration distance of the compound is proportional to that of the solvent. As the result, the R, value of any compound is obtained with excellent reproducibility.
In addition, as the plates can be suspended with clips from some horizontal bars fixed up to the support means, a plurality of plates can be used for development, and raised or lowered smoothly.
Furthermore, there are two advantages as follows from such suspending system: (1) The lower edge of the plate can be immersed into the solvent to a desired depth even on the condition in which a large quantity of solvent has been put in the chamber. Without exchanging the solvent in the chamber as far as the constituent of the solvent does not change, thin-layer chromatography is performed to continue for the same purpose. (2) The bottom of the chamber used need not be flat.
The invention will be described hereinafter with reference to the annexed drawing, in which FIG. 1 is the front view of the mode of an embodiment of this invention.
FIG. 2 is the cross sectional view of FIG. 1.
. FIG. 3 is the cross sectional view of the second embodiment of this invention, and
FIG. 4 is the drawing of the patterns wherein the distance of movement of a substance is shown by the longitudinal axis and the distance of permeation of solvent is shown by the transversal axis.
As shown in FIGS. 1 and 2, the solvent chamber 10 is made of glass, and in the shape of a somewhat deep box whose top is opened; its edge 11 is finished smooth so that its interior can be tightly shut with a cover 12.
The cover 12 is very tight and the support means 13 which also serves as a knob is fixed up approximately at the center of the cover. Said support means 13 is composed of a guide pipe 14 fixed, a rod 15 inserted through the interior of the guide pipe 14 and a nut 17 screwed up to the screw part 16 of the rod 15.
As shown in FIG. 2, a lower part of the guide pipe 14 is screwed up, and fixed with two ring nuts 18 and 19 from inside and outside of the cover 12, through a hole at the center of the cover.
The rod 15 is inserted through the interior of the guide pipe and can be rised and lowered byturning a ring 17.
If necessary, a packing and other suitable sealing means may be put on the top of the guide pipe in order that solvent vapor in the interior of the solvent chamber 10 may not leak out of the space between the top of the guide pipe and a lower part of the ring 17.
At the lower end of the rod 15 is formed a screw 26, which is screwed up to the screw hole of an arm 20, and the rod 15 is vertically equipped at a right angle to the arm 20. At two sides of the arm 20 there are made a plurality of (four shown in the drawing) screw holes at intervals in the horizontal direction, and into each screw hole 22 there is fixed up a horizontal bar 21, from which the plate 24 of development is suspended by means of a clip 23. The horizontal bars 21 are supported in parallel with one another. The support means, arm and horizontal bars are made of a stainless steel or plastic materials that remain uneffected by several organic solvent, acids or alkali.
Furthermore, it is also sufficient that ordinary holes are made on the arm 20 instead of a plurality of screw holes and a horizontal bar is inserted through each of the ordinary holes. 7
There are different sizes of chromatoplates such as 5 X 10cm, 5 X 20cm, 20 X 20cm etc., and the embodiments shown in FIG. 1 and 2 respectively show a case in which each of two plates having the size of 20 X 20cm is suspended by means of each of two horizontal bars 21. Of course, it is also possible that each of a required number of the plates having different sizes is suspended by means of each horizontal bar. However, as for plates having such a short length as the 5 x IOcm-type, it is sufficient that the rod 15 in the support means is replaced by an enormous rod or one enlarged by'connecting some joints 25a and 25b having a screw 36 respectively which is conjugated to the lower part of the rod 15 as shown in FIG. 3 so that the rod may have a required length.
Besides, if the equilibration of each horizontal bar is difficult to keep only by the arm 20, it is sufficient that a guide member (not shown) having the same shape as that of the support arm 20, is inserted into one end of each horizontal bar 21 and through the bar in order that the equilibration may be kept by regulating the distance between the horizontal bars 21.
After a spot of a substance to be examined is applied to the plate for development 24, the plate is suspended from a horizontal bar 21 with the clip 23, and without immersing the plate into the solvent setinto the solvent chamber 10, in which amount of solvent 30 necessary for development has been put into the solvent chamber in advance. After the equilibration of the plate with solvent vaporis completely achieved in the chamber, the plate 24 for development is immersed into the solvent chamber by turning and adjusting the nut 17 of the support means and thus developed with the solvent 30. The rod of the support means 13 is made to rise, and the lower end of the plate 24 is kept from soaking in the solvent 30 in the solvent chamber. Namely, as the lower end of the plate 24 is distant from the solvent, in this condition there is no movement of any substance on the plate and development is not yet made.
As a cover 12 is put on the top of the solvent chamber, solvent vapor forms its saturation after a while. After observing this, an adjusting nut 17 of the support means is loosened and the rod is made to slide downward so that the lower end of the developing plate 24 can be made to soak in the liquid layer of the solvent 30. In this way, the developing doesn't start till the developing plate 24 is made to fall and touch the solvent liquid. At this time, any substance and the solvent move very briskly, as vaporization of the solvent from the plate does not occur because of saturation of the chamber, and, in addition, as shown in a thick line in FIG. 4, the distance of movement of the substance is in right proportion to the distance of permeation of the solvent, so that a straight-line for development curve of any substance is drawn.
As seen from FIG. 4, the development curve of a compound is straight-line according to this invention, and especially at the initial stage of the development high precision can be obtained as compared with a conventional method. Two thin and dotted lines shown in FIG. 4, show curves obtained when some compounds,
one of which was different from the above compound, had been developed.
Besides, in the embodiments of this invention, 1 described about thin-layer chromatography, and it is needless to say that this invention canbe applied to paper-chromatography too.
I claim:
1. A device for deveopment in thin-layer chromatography comprising a solvent container, an air tight cover for said container, said container and cover defining an airtight chamber in which a quantity of liquid solvent is disposed, said chamber above said liquid solvent being saturated with said solvent, support means mounted on said cover and extending into said chamber, said support means suspending at least one developing plate within said solvent chamber, and actuating means operatively connected to said support means and actuable externally of said solvent chamber for raising and lowering said support means within said chamber, whereby said developing plate is subjected to the saturated solvent within said chamber above said quantity of liquid solvent before being lowered for immersion into said liquid solvent.
2. Apparatus according to claim 1 wherein said cover has an opening, said support means comprising a guide tube mounted in said opening, a rod mounted in said guide tube, a rotary element disposed externally of said cover and operably with said rod to raise and lower the latter, and support elements within. said enclosure mounted on said rod for holding said developing plate in a suspended disposition, whereby rotation of said externally mounted rotary element lowers said development plate.
3. Apparatus according to claim 2 wherein said rod is provided with extension means, said support elements being mounted on said extension means, thereby adapting said apparatus for handling shorter developing plates.
4. Apparatus according to claim 2 wherein clips are provided on said support elements, said development plates being suspended by said clips.
5. Apparatus according to claim 4 wherein said clips are made of polyacetal resin.
patent 3,752, 316 Dated August 14, 1973 Inventor(s) Ryuzo hlta It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
In the heading of the patent, the address of the inventor should read:
-No. 5-4-11, Koenji Minami, SuginaQmi-ku,
Tokyo, Japan-.
Signed and sealed this 23rd day of April 1971],.
(SEAL) Attest:
EDI-IARD PLFLETCHEILJR. C MARSHALL DAMN Attesting Officer Commissioner of Patents ORM PO-105O (10-69) usco M-Dc 60376-P69 w u. s. aovsmmzm' rnm'nua OFFICE 1 I!" o-aee-azu,

Claims (5)

1. A device for deveopment in thin-layer chromatography comprising a solvent container, an air tight cover for said container, said container and cover defining an airtight chamber in which a quantity of liquid solvent is disposed, said chamber above said liquid solvent being saturated with said solvent, support means mounted on said cover and extending into said chamber, said support means suspending at least one developing plate within said solvent chamber, and actuating means operatively connected to said support means and actuable externally of said solvent chamber for raising and lowering said support means within said chamber, whereby said developing plate is subjected to the saturated solvent within said chamber above said quantity of liquid solvent before being lowered for immersion into said liquid solvent.
2. Apparatus according to claim 1 wherein said cover has an opening, said support means comprising a guide tube mounted in said opening, a rod mounted in said guide tube, a rotary element disposed externally of said cover and operably with said rod to raise and lower the latter, and support elements within said enclosure mounted on said rod for holding said developing plate in a suspended disposition, whereby rotation of said externally mounted rotary element lowers said development plate.
3. Apparatus according to claim 2 wherein said rod is provided with extension means, said support elements being mounted on said extension means, thereby adapting said apparatus for handling shorter developing plates.
4. Apparatus according to claim 2 wherein clips are provided on said support elements, said development plates being suspended by said clips.
5. Apparatus according to claim 4 wherein said clips are made of polyacetal resin.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5152177A (en) * 1990-09-07 1992-10-06 Conoco Inc. Process for the detection and quantitation of corrosion and scale inhibitors in produced well fluids
US5350510A (en) * 1993-02-11 1994-09-27 Granite Engineering, Inc. Apparatus for thin layer chromatography
WO2000062055A1 (en) * 1999-04-13 2000-10-19 Markoski Larry J Method and apparatus for developing multiple thin layer chromatography plates
US20030013187A1 (en) * 2000-02-14 2003-01-16 Rolf Guller Device for analyzing substances by means of thin layer chromatography
US20040241051A1 (en) * 2000-10-25 2004-12-02 Steag Microparts Structures for uniform capillary flow
CN109490463A (en) * 2018-11-12 2019-03-19 安徽中医药高等专科学校 A kind of chromatography teaching aid and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3341017A (en) * 1965-02-23 1967-09-12 Shandon Scient Company Ltd Chromatographic apparatus
US3342333A (en) * 1963-01-11 1967-09-19 Europ Atomic Energy Communtiy Apparatus for thin-layer chromatography

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3342333A (en) * 1963-01-11 1967-09-19 Europ Atomic Energy Communtiy Apparatus for thin-layer chromatography
US3341017A (en) * 1965-02-23 1967-09-12 Shandon Scient Company Ltd Chromatographic apparatus

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5152177A (en) * 1990-09-07 1992-10-06 Conoco Inc. Process for the detection and quantitation of corrosion and scale inhibitors in produced well fluids
US5350510A (en) * 1993-02-11 1994-09-27 Granite Engineering, Inc. Apparatus for thin layer chromatography
US6264893B1 (en) 1998-04-13 2001-07-24 Larry J. Markoski Method and apparatus for developing thin layer chromatography plates for maximizing mobile phase conditions in column chromatography
WO2000062055A1 (en) * 1999-04-13 2000-10-19 Markoski Larry J Method and apparatus for developing multiple thin layer chromatography plates
US20030013187A1 (en) * 2000-02-14 2003-01-16 Rolf Guller Device for analyzing substances by means of thin layer chromatography
US6709584B2 (en) * 2000-02-14 2004-03-23 Chemspeed Ltd. Device for analyzing substances by means of thin layer chromatography
US20040241051A1 (en) * 2000-10-25 2004-12-02 Steag Microparts Structures for uniform capillary flow
US8231845B2 (en) * 2000-10-25 2012-07-31 Steag Microparts Structures for uniform capillary flow
CN109490463A (en) * 2018-11-12 2019-03-19 安徽中医药高等专科学校 A kind of chromatography teaching aid and preparation method thereof

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