GB2029813A - Ceramic Body for Chromatography - Google Patents
Ceramic Body for Chromatography Download PDFInfo
- Publication number
- GB2029813A GB2029813A GB7926130A GB7926130A GB2029813A GB 2029813 A GB2029813 A GB 2029813A GB 7926130 A GB7926130 A GB 7926130A GB 7926130 A GB7926130 A GB 7926130A GB 2029813 A GB2029813 A GB 2029813A
- Authority
- GB
- United Kingdom
- Prior art keywords
- ceramic body
- chromatography
- alumina
- sheet
- thin layer
- Prior art date
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- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 31
- 238000009826 distribution Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000011148 porous material Substances 0.000 claims abstract description 11
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 20
- 230000005526 G1 to G0 transition Effects 0.000 claims description 17
- 238000001354 calcination Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 11
- 238000004817 gas chromatography Methods 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 239000007788 liquid Substances 0.000 description 11
- 238000000926 separation method Methods 0.000 description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical compound CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 description 6
- 238000004811 liquid chromatography Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- 239000004793 Polystyrene Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 229920002223 polystyrene Polymers 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 3
- 239000004395 L-leucine Substances 0.000 description 3
- 235000019454 L-leucine Nutrition 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Chemical compound CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 description 3
- 229940024606 amino acid Drugs 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229960003136 leucine Drugs 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- 239000004945 silicone rubber Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 description 2
- JCYPECIVGRXBMO-UHFFFAOYSA-N 4-(dimethylamino)azobenzene Chemical compound C1=CC(N(C)C)=CC=C1N=NC1=CC=CC=C1 JCYPECIVGRXBMO-UHFFFAOYSA-N 0.000 description 2
- QNAYBMKLOCPYGJ-UHFFFAOYSA-N Alanine Chemical compound CC([NH3+])C([O-])=O QNAYBMKLOCPYGJ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GUBGYTABKSRVRQ-DCSYEGIMSA-N Beta-Lactose Chemical compound OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-DCSYEGIMSA-N 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- CZMRCDWAGMRECN-FBXJDJJESA-N D-sucrose Chemical compound O[C@@H]1[C@@H](O)[C@H](CO)O[C@]1(CO)O[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](CO)O1 CZMRCDWAGMRECN-FBXJDJJESA-N 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 2
- LKDRXBCSQODPBY-AMVSKUEXSA-N L-(-)-Sorbose Chemical compound OCC1(O)OC[C@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-AMVSKUEXSA-N 0.000 description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N L-sorbitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- NNBZCPXTIHJBJL-AOOOYVTPSA-N cis-decalin Chemical compound C1CCC[C@H]2CCCC[C@H]21 NNBZCPXTIHJBJL-AOOOYVTPSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001030 gas--liquid chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229940078552 o-xylene Drugs 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- VRZJGENLTNRAIG-UHFFFAOYSA-N 4-[4-(dimethylamino)phenyl]iminonaphthalen-1-one Chemical compound C1=CC(N(C)C)=CC=C1N=C1C2=CC=CC=C2C(=O)C=C1 VRZJGENLTNRAIG-UHFFFAOYSA-N 0.000 description 1
- BYFGZMCJNACEKR-UHFFFAOYSA-N Al2O Inorganic materials [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 241000206607 Porphyra umbilicalis Species 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003849 aromatic solvent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000574 gas--solid chromatography Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- NNBZCPXTIHJBJL-UHFFFAOYSA-N trans-decahydronaphthalene Natural products C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 1
- NNBZCPXTIHJBJL-MGCOHNPYSA-N trans-decalin Chemical compound C1CCC[C@@H]2CCCC[C@H]21 NNBZCPXTIHJBJL-MGCOHNPYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- 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
- G01N30/92—Construction of the plate
- G01N30/93—Application of the sorbent layer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
Abstract
A ceramic body for chromatography consists of a calcined molded body of alumina particles composed mainly of alpha -alumina, preferably containing a minor amount (less than 50 wt %) of gamma - alumina, and which has a narrow pore size distribution range (0.1 to 10 microns). A process for making the ceramic body is disclosed. This ceramic body has no substantial adsorbing property and therefore, when it is used in thin layer chromatography (as a molded plate) or gas chromagraphy (after pulverising), the tailing phenomenon does not occur and a high separating capacity can be obtained.
Description
SPECIFICATION
Ceramic Body for Chromatography and Process for Preparation Thereof
This invention relates to a ceramic body for chromatography consisting of a calcined molded body of a-alumina particles. More particularly, the invention relates to a ceramic body which exerts a high and stable separating capacity without substantial occurrence of the tailing phenomenon when it is used for use like to thin layer chromatography or gas chromatography.
Chromatography is broadly used in the fields of biochemistry, manufacture of agricultural chemicals, manufacture of medicines and other various chemical industries as a process in which a sample is separated to the respective components by utilizing adsorption and/or distribution.
The chromatography heretofore adopted in these fields is roughly divided into two types, that is, the adsorption type and distribution type. Thin layer chromatography is a typical instance of the chromatography utilizing the principles of both the adsorption type and distribution type, and a typical instance of the chromatography utilizing the principle of the distribution type is liquid chromatography.
In the thin layer chromatography, a mixture formed by kneading an inorganic or organic adsorbent such as silica. gel, alumina or polyamide with a binder, water and other appropriate components with the use of a mixing solvent is coated in the form of a thin layer on a plate-like support such as a glass sheet, a synthetic resin sheet or a metal sheet, the coated mixture is dried under predetermined conditions, an unknown sample is dropped on one end of the thin layer, the lower end or upper end of the plate-like support is dipped in the solvent while the solvent is being evaporated, and after a certain developing time, adsorption and separation of the sample are repeated while the solvent is passed through the thin layer by the capillary phenomenon. By utilizing this phenomenon of the repeated adsorption and separation of the sample, the unknown sample is separated and analyzed.
In the thin layer chromatography, an expensive equipment for formation of a thin layer, such as an applicator, must be used and a considerable skill is necessary for forming a thin layer by using such equipment. Furthermore, a thin layer having a uniform thickness can hardly be obtained. If the thickness of the thin layer is not uniform, attainment of uniform development is very difficult and the result of development lacks reliability and reproducibility. Moreover, even if thin lavers are composed of the same material, the activity differs depending on the degree of drying of the adsorbent. Still further, it is very difficult to prepare a number of thin layers continuously, and since a thin layer is formed on a glass substrate or the like by coating, the thin layer is readily peeled by vibration or the like during transportation.Thus, the conventional technique of thin layer chromatography includes various defects.
The liquid chromatography where a substance having a large distribution coefficient is separated and eluted out preferentially is a typical instance of the distribution type chromatography. More specifically, it is necessary to inject a minute amount of a liquid sample into a carrier liquid before a column against the pressure of the carrier liquid (for example, 300 atmospheres) promptly and preciseiy. In the conventional piercing cap technique using a piston type injection mechanism for the injection, since the inner pressure of the carrier liquid is high, the reproducibility is not always good.
Moreover, different materials should be chosen and used for piercing caps according to the intended object of chromatography. Furthermore, when a fine tube of the injection device is introduced into the carrier liquid, a shock pressure is generated because of the non-compressibility of the carrier liquid and this shock pressure is transmitted to the column and detector, and the analysis process is susceptively influenced. In such liquid chromatography, the amount to be developed at one time is small and if the sample is not diluted, the separation capacity is degraded. Therefore, the liquid-phase chromatography is defective in that it takes a long time to separate and collect the sample in an amount necessary for analysis or the like. Furthermore, it is difficult to pack the stationary layer uniformly in a column and commercially available products are very expensive.Moreover, the liquid chromatography is disadvantageous in that detection must be conducted on separation and collection by such means as ultraviolet analysis or refractive index analysis and the entire equipment system becomes voluminous, and that the equipment system must be washed sufficiently before and after separation and collection.
As will be apparent from the foregoing illustration, the conventional chromatography of either the adsorption type or the distribution type involves various defects with respect to the separation capacity and the operation procedures.
In gas chromatography, a gaseous sample or gasified liquid or solid sample is passed through a tube uniformly packed with a filler and thus developed by means of a carrier gas and the sample is separated into respective components. This gas chromatography is roughly divided into gas-solid chromatography where a solid power having an adsorbing capacity is used as the filler and the respective components are separated by utilizing the difference of the adsorbing property and gasliquid chromatography where a lowly volatile liquid or a solid to be liquefied at the application temperature is used as the filler and the respective components are separated by utilizing the difference of the solubility.
Celite or the like having no adsorbing activity is ordinarily used as a carrier of the stationary phase in the above-mentioned gas-liquid chromatography, and conventional alumina cannot be used for this purpose because the adsorbing activity is very high and tailing is readily caused.
According to this invention, there is provided a ceramic body for chromatography which have chemical structure and characteristics quite different from alumina heretofore used as the adsorbing medium or stationary phase in chromatography.
More specifically, in accordance with this invention, there is provided a ceramic body for chromatography, which consists of a calcined and molded body of crystalline alumina particles composed mainly of a-alumina and which has a narrow pore size distribution range.
Since the ceramic body for chromatography according to this invention has no substantial adsorbing property, the tailing phenomenon is not substantially caused when materials are separated, and the high separation capacity can be attained very stably.
Still further, this ceramic body for chromatography can be provided very easily at a low cost only by molding and calcining alumina particles composed mainly of alumina. Furthermore, the ceramic body for chromatography according to this invention is very excellent in the mechanical strength, the easiness in handling and the adaptability to the analysis operation.
This invention will now be described in detail by reference to the accompanying drawings, in which:
Figure 1 is a diagram illustrating the state where sugars are separated by using a sheet-like ceramic body for chromatography according to this invention,
Figures 2 and 3 are diagrams illustrating the state where amino acids are separated by using a sheet-like ceramic body four chromatography according to this invention.
Figure 4 is a diagram illustrating the state where oil soluble dyes are separated by using a sheetlike ceramic body for chromatography according to this invention,
Figure 5 is a diagram illustrating the state where polystyrenes having various molecular weights are separated by using a sheet-like ceramic body for chromatography according to this invention,
Figure 6 is a graph illustrating a relation between the developing distance and the molecular weight in the chromatogram of Figure 5,
Figures 7 and 8 are diagrams illustrating results of separation of samples by using a stationary phase carrier for gas chromatography according to this invention.
In this invention, crystalline alumina particles composed mainly of a-Al2O are used as the starting material. Of course, alumina particles composed solely of a-A1203 may be used, but when alumina particles comprising more than 50% by weight, preferably 60 to 80% by weight, of cr-AI203 and less than 50% by weight, preferably 20 to 40% by weight, of y-alumina are used, an optimum separation capacity can be obtained.
Alumina particles having an average particle size smaller than 30 y and a narrow particle size distribution range are preferred. Optimum results can be obtained when alumina particles having a particle size distribution range of from 1 to 10 ,u are employed.
The ceramic body of this invention can be prepared according to a process comprising molding a composition comprising crystalline alumina particles composed mainly of alumina, a resinous binder and a solvent into the form of a sheet, calcining the molded sheet at a temperature of 850 to 16000 C.
and, if necessary, pulverizing the calcined sheet into particles.
An acrylic resin or polyvinyl butyral (PVB) is preferably used as the resinous binder. Furthermore, polyvinyl acetate, polyesters and other resinous binders may be used in this invention. Aromatic solvents such as toluene and xylene, alcohols such as methanol and ethanol, ketones such as acetone and methylethyl ketone and the like can optionally be used as the solvent.
The amount used of the resinous binder is selected so that the obtained sheet is good for the mechanical processing, and the amount used of the solvent is selected so that the surfaces of alumina particles are sufficiently wetted and a flowability necessary for molding is obtained.
The above-mentioned composition is made homogeneous by agitation, kneading or the like, and the homogeneous composition is molded into a predetermined shape, ordinarily a planar shape, for example, a tape or sheet, by tape casting using a doctor blade.
The molded sheet is calcined at a temperature of 850 to 16000 C., whereby particles of a-Al203 are partially fused to one another and integrated with one another to obtain a microporous molded body. A prefered calcination temperature differs to some extent depending on the kind of chromatography. For example, in case of liquid chromatography, a calcination temperature of 1250 to 1 4000C. is preferred and in case of the stationary phase carrier for gas chromatography, a calcination temperature of 1 150 to 1 4000C. is preferred.
This calcined sheet has a narrow pore size distribution range, and it is preferred that the pore size distribution range be substantially from 0.1 to 10 ,u.
The obtained calcined and molded sheet is used as a ceramic body for liquid chromatography as it is or after it has been cut in a predetermined size according to need.
This calcined and molded sheet is used as a stationary phase carrier for gas chromatography after it has been pulverized into particles and if necessary, the particle size has been adjusted.
This invention will now be described in detail by reference to the following Examples that by no means limit the scope of the invention.
Example 1
Starting a-Al2O3 particles having the average particle size of 1 to 2 ssu were used. Then, 100 parts by weight of the starting material were mixed with 8 parts by weight, as the solids, of an acrylic resin and 40 parts by weight of toluene as the solvent. The resulting composition was kneaded and molded into a tape having a thickness of 1 mm by using a doctor blade.
Plates having a size of 1.5 cmxl 0 cm were cut from the so molded tape and calcined at 850,
1285, 1390 or 1 6000C., and the relation between the calcination temperature and the developing speed was examined. Results obtained when n-hexane was used as a developing liquid are shown in
Table 1.
Table 1
Developing
Run No. Calcination Temperature (0C.) Time (mien) 1 850 16
2 1285 25
3 1390 30
4 1600 42
Note
The developing distance of the solvent was 6.0 cm in each run.
The ceramic body obtained by carrying out calcination at 8500C. showed a shortest developing
time, i.e., 1 6 minutes, among the so-obtained calcined ceramic bodies, but from the viewpoint of the
strength of the ceramic body for chromatography, the ceramic body obtained by carrying out
calcination at 1 2850C. was most preferred. Accordingly, the ceramic body formed by carrying out
calcination at 1 2850C. was cut into strips and subjected to the experiments described in Examples 2
and 3 given below.
Example 2 (Sugars)
D(+)-lactose, D(+)-sucrose and L(-)-sorbose and a mixture thereof were developed with a
mixture of water/ethyl acetate/n-propanol (1/35/10 in VolumeNolume ratio) by using the sheet-like
ceramic body of Example 1. Coloration was performed by using sulfuric acid. Results obtained were
shown in Figure 1.
In Figure 1, (a), (b), (c) and (mix) stand for D(+)-lactose, D(+)-sucrose, L(-)-sorbose and mixture
thereof respectively.
Example 3 (Amino Acid)
Results where glycine, D,L-alanine, D,L-valine and L-leucine were developed by using the sheet
like ceramic body of Example 1 were shown in Figure 2. A mixture of water/ethyl acetate/n-propanol
(5/35/10 in volume/volume ratio) was used as developer, and ninhydrin was used for coloration. In
Figure 2 and Figure 3 as mentioned below, (i), (ii), (iii) and (iv) stand for glycine, D,L-alanine, D,L-valine
and L-leucine respectively.
As will be apparent from the foregoing illustration, in this invention, since a-AI203 which is very
stable and has no substantial adsorbing property is used as the ceramic body for chromatography,
substances can be clearly separated based on the difference of the distribution coefficient.
Characteristic properties of the ceramic body for chromatography according to this invention are as follows.
(1) Since a-AI203 has a very low activity and is very stable, the ceramic body exerts no substantial
adsorbing property, and the ceramic body can be applied to systems to which only liquid-phase
chromatography has heretofore been applied.
(2) Large quantities of samples can be separated in a short time very simply.
(3) Since alumina uniform in the particle size is molded by using a binder in the ceramic body of this invention, a uniform thickness can be obtained and the resulting ceramic body is excellent in the
separating capacity and reproducibility.
(4) Since calcination is carried out after molding, the mechanical strength is high and deformation
is not caused in the ceramic body of this invention.
(5) Desorption can easily be accomplished only by cutting off the portion used for separation and
treating it with a solvent capable of dissolving the separated component sufficiently.
(6) Since molding can be performed continuously, the manufacturing cost can be remarkably
reduced.
Example 4
A sheet-like ceramic body was prepared in the same manner as described in Example 1 except that a-Al2O3 and y-AI203 were used in combination at a weight ratio of 75/25 instead of the a-Al203 used in Example 1 and calcination was carried out at 1 3500C.
Amino acids were separated in the same manner as described in Example 3 by using the so prepared sheet-like ceramic body. Obtained results are shown in Figure 3, from which it will readily be understood that even in the case of substances having a relatively low Rf value D,L-valine, L-leucine, occurrence of the tailing phenomenon could be completely inhibited and each spot was very clear.
Example 5 (Oil-soluble Dyestuff)
A mixture of Indophenol Blue (I), Sudan Red (II) and 4-Dimethylaminoazobenzene (Ill) was developed with n-hexane by using the ceramic body of Example 4. The results obtained were shown in
Figure 4, from which it will be understood that each spot was very clear and occurrence of the tailing
phenomenon could be completely inhibited.
Example 6 (Polystyrene)
Results were 4 kinds of polystyrene having an average molecular weight (MW) of 2,000, 20,000,
160,000 and 1,800,000 respectively were developed with tetrahydrofuran (THF) and ethanol (15:11 in volume ratio) by using the sheet-like ceramic substance were shown in Figure 5. lode was used for coloration. The relation between the molecular weight of polystyrene and the developing distance were shown in Figure 6 from which it will be understood that there is established a linear relation between the developing distance and the molecualr weight and that the molecular weight of polymer can be estimated from this relation.
Example 7
High-purity alumina (AI2O3) was molten in an electric furnace and was then solidified. The resulting mass was pulverized and classified to obtain a white corundum crystalline powder having a particle size distribution range of from 0.5 to 80 u and an average particle size of 10 Ju (30 ,u).
Then, 100 parts by weight of the so formed crystalline powder was mixed with 20 to 60 parts by weight (preferably 30 to 50 parts by weight) of toluene as the organic solvent, and the mixture was sufficiently stirred in a pot mill. Then, the mixture was mixed with 4 to 40 parts by weight (preferably 6 to 15 parts by weight) of an acrylic resin as the binder, and the mixture was sufficiently stirred. Then, the mixture was molded into a green ceramic tape having a uniform thickness of 0.2 to 2.0 mm (preferably 0.25 to 1.0 mm) according to the doctor blade method.The green tape was cut into a predetermined size and calcined at 1000 to 1 6000C. (preferably 1200 to 1 3500C.) to obtain a sheetlike ceramic body having a pore size of 0.1 to 10 y. The sheet-like ceramic body was pulverized in a mortar and a fraction of 60 to 80 mesh was collected. Then, 22 g of the so obtained powder was dipped in a solution of 0.7 g of a silicone rubber in 1 5 cc of tetrahydrofuran (hereinafter referred to as "THF"). THF was evaporated while the mixture was quietly agitated by a spatula, whereby a stationary phase was obtained.
The so prepared stationary phase for gas chromatography was packed in a column having a length of 2 m, and experiments described in Examples 8 and 9 were carried out by using the so prepared packed column.
Example 8
A mixture containing benzene, toluene and o-xylene at a volume ratio of 1/1/1 was separated under the following conditions:
Flow rate: 29.2 ml/min
Amount injected: 3,ul Column pressure: 0.8 Kg/cm2 Temperature: 1 300C.
Carrier gas: nitrogen (N2) gas
Stationary phase liquid: silicone rubber
Detection method: TCD (thermal conductivity detector) method
Obtained results are shown in Figure 8. As will be apparent from the graph of Figure 8, sharp peaks corresponding to the separated substances were detected, and the presence of benzene, toluene and o-xylene could be clearly confirmed at points A, B and C, respectively.
Example 9
A mixture of dioxane, butyl acetate, isobutyl ketone, trans-decalin and cis-decalin was separated under the following conditions:
Flow rate: 30 ml/min
Amount injected: 5 ,us Column pressure: 0.7 Kg/cm2
Temperature: 1 300C.
Carrier gas: nitrogen (N2) gas
Stationary phase liquid: silicone rubber
Detection method: TCD method
Obtained results are shown in Figure 8. As will be apparent from the graph of Figure 8, sharp peaks corresponding to the respective substances were observed. More specifically, the presence of dioxane, butyl acetate, isobutyl ketone and cis-decalin could be confirmed at points D, E, F and G, respectively.
It was found that if the pore size exceeds 10,u, separation of the respective components becomes difficult.
As will be apparent from the foregoing illustration, since alumina having a uniform crystal particle size is used for the stationary phase carrier for gas chromatography according to this invention, the stationary phase carrier has no substantial adsorbing property and hence, the tailing phenomenon is not caused to occur at all. Moreover, since the bulk density of the stationary phase carrier alumina of this invention is higher than that of celite customarily used in this field, the time required for packing can be shortened to about 5 minutes (several hours are necessary in case of conventional celite).
Moreover, since the stationary phase carrier of this invention is hard and hardly pulverizabie, it is not broken or divided when the column is wound in the spiral form. Furthermore, since the stationary phase carrier of this invention is prepared by calcining a molded body having a tape-like shape and pulverizing the calcined body, the pore size distribution range (the range of sizes of pores among crystal particles) is very narrow, that is from 0.1 to 10 , and therefore, the resulting stationary phase carrier can exert an excellent separating capacity very stably.
Claims (11)
1. A ceramic body for use in chromatography which consists of a calcined and molded body of alumina particles composed mainly of alumina and has a narrow pore size distribution range.
2. A ceramic body according to claim 1 wherein the alumina particles comprise more than 50% by weight of alumina and less than 50% by weight of y-alumina.
3. A ceramic body according to claim 1 or 2 wherein the alumina particles have a particle size not exceeding 30 y.
4. A ceramic body according to claim 1,2 or 3 wherein the calcined and molded body has pores having a pore size of from 0.1 to 10
5. A ceramic body according to any one of the preceding claims wherein the molded body is in the form of a sheet and is suitable for use in thin layer chromatography.
6. A ceramic body according to any one of claims 1 to 4 wherein the molded body is in particulate form and is suitable for use as the stationary phase carrier in gas chromatography.
7. A ceramic body according to claim 1 substantially as described in any one of the Examples.
8. A process for the preparation of a ceramic body as claimed in any one of the preceding claims, which process comprises molding a composition comprising the alumina particles, a resinous binder and a solvent into the form of a sheet, and calcining the molded sheet at a temperature of 850 to 16000C.
9. A process according to claim 8 wherein the calcined sheet is pulverized into particles.
10. A process according to claim 8 substantially as described in any one of the Examples.
11. Use of a ceramic body as claimed in any one of claims 1 to 7 as the thin layer in thin layer chromatography or as a stationary phase carrier in gas chromatography.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP53092384A JPS6041018B2 (en) | 1978-07-27 | 1978-07-27 | Ceramic body for chromatography |
| JP5443879A JPS55146039A (en) | 1979-05-02 | 1979-05-02 | Stationary phase carrier for gas chromatography |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2029813A true GB2029813A (en) | 1980-03-26 |
| GB2029813B GB2029813B (en) | 1982-12-08 |
Family
ID=26395198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB7926130A Expired GB2029813B (en) | 1978-07-27 | 1979-07-26 | Ceramic body for chromoatography |
Country Status (6)
| Country | Link |
|---|---|
| CA (1) | CA1139588A (en) |
| DE (1) | DE2930585A1 (en) |
| FR (1) | FR2435448A1 (en) |
| GB (1) | GB2029813B (en) |
| IT (1) | IT1123488B (en) |
| NL (1) | NL7905805A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018011180A1 (en) * | 2016-07-14 | 2018-01-18 | Akzo Nobel Chemicals International B.V. | Building composition marker |
| WO2018011178A1 (en) * | 2016-07-14 | 2018-01-18 | Akzo Nobel Chemicals International B.V. | Etics mortar composition |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE9405378U1 (en) * | 1994-03-30 | 1994-06-23 | Hewlett-Packard GmbH, 71034 Böblingen | Separation column for chromatography |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1417557A (en) * | 1963-12-14 | 1965-11-12 | Merck Ag E | Adsorbent suitable for plate chromatography |
-
1979
- 1979-07-25 FR FR7919210A patent/FR2435448A1/en active Granted
- 1979-07-26 NL NL7905805A patent/NL7905805A/en not_active Application Discontinuation
- 1979-07-26 IT IT24719/79A patent/IT1123488B/en active
- 1979-07-26 CA CA000332574A patent/CA1139588A/en not_active Expired
- 1979-07-26 GB GB7926130A patent/GB2029813B/en not_active Expired
- 1979-07-27 DE DE19792930585 patent/DE2930585A1/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018011180A1 (en) * | 2016-07-14 | 2018-01-18 | Akzo Nobel Chemicals International B.V. | Building composition marker |
| WO2018011178A1 (en) * | 2016-07-14 | 2018-01-18 | Akzo Nobel Chemicals International B.V. | Etics mortar composition |
| US10766816B2 (en) | 2016-07-14 | 2020-09-08 | Nouryon Chemicals International B.V. | Building composition marker |
Also Published As
| Publication number | Publication date |
|---|---|
| IT7924719A0 (en) | 1979-07-26 |
| FR2435448A1 (en) | 1980-04-04 |
| IT1123488B (en) | 1986-04-30 |
| CA1139588A (en) | 1983-01-18 |
| NL7905805A (en) | 1980-01-29 |
| GB2029813B (en) | 1982-12-08 |
| FR2435448B1 (en) | 1983-12-02 |
| DE2930585A1 (en) | 1980-02-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |