JPH03165260A - Plate for thin-layer chromatography and production thereof - Google Patents
Plate for thin-layer chromatography and production thereofInfo
- Publication number
- JPH03165260A JPH03165260A JP1305580A JP30558089A JPH03165260A JP H03165260 A JPH03165260 A JP H03165260A JP 1305580 A JP1305580 A JP 1305580A JP 30558089 A JP30558089 A JP 30558089A JP H03165260 A JPH03165260 A JP H03165260A
- Authority
- JP
- Japan
- Prior art keywords
- metal oxide
- oxide film
- plate
- layer chromatography
- thin layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004809 thin layer chromatography Methods 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 47
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims description 34
- 230000007261 regionalization Effects 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 238000004040 coloring Methods 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000004451 qualitative analysis Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 32
- 239000000047 product Substances 0.000 description 16
- 239000003463 adsorbent Substances 0.000 description 13
- 239000011347 resin Substances 0.000 description 13
- 229920005989 resin Polymers 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000011521 glass Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000004925 Acrylic resin Substances 0.000 description 7
- 229920000178 Acrylic resin Polymers 0.000 description 7
- 239000001045 blue dye Substances 0.000 description 7
- -1 Yztrium Chemical compound 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000000975 dye Substances 0.000 description 5
- 238000010894 electron beam technology Methods 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- OXLITIGRBOEDEZ-UHFFFAOYSA-N 1,5-diamino-4,8-dihydroxy-2-(4-hydroxyphenyl)anthracene-9,10-dione Chemical compound C=1C(O)=C2C(=O)C=3C(N)=CC=C(O)C=3C(=O)C2=C(N)C=1C1=CC=C(O)C=C1 OXLITIGRBOEDEZ-UHFFFAOYSA-N 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000005388 borosilicate glass Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920003986 novolac Polymers 0.000 description 2
- 239000001048 orange dye Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000001047 purple dye Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- IBABXJRXGSAJLQ-UHFFFAOYSA-N 1,4-bis(2,6-diethyl-4-methylanilino)anthracene-9,10-dione Chemical compound CCC1=CC(C)=CC(CC)=C1NC(C=1C(=O)C2=CC=CC=C2C(=O)C=11)=CC=C1NC1=C(CC)C=C(C)C=C1CC IBABXJRXGSAJLQ-UHFFFAOYSA-N 0.000 description 1
- MHXFWEJMQVIWDH-UHFFFAOYSA-N 1-amino-4-hydroxy-2-phenoxyanthracene-9,10-dione Chemical compound C1=C(O)C=2C(=O)C3=CC=CC=C3C(=O)C=2C(N)=C1OC1=CC=CC=C1 MHXFWEJMQVIWDH-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 239000013032 Hydrocarbon resin Substances 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- WVVOBOZHTQJXPB-UHFFFAOYSA-N N-anilino-N-nitronitramide Chemical compound [N+](=O)([O-])N(NC1=CC=CC=C1)[N+](=O)[O-] WVVOBOZHTQJXPB-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- NDYFZEOTGYVXNJ-UHFFFAOYSA-N [Zn].[Zn][Sn] Chemical compound [Zn].[Zn][Sn] NDYFZEOTGYVXNJ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000000981 basic dye Substances 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- ISRJTGUYHVPAOR-UHFFFAOYSA-N dihydrodicyclopentadienyl acrylate Chemical compound C1CC2C3C(OC(=O)C=C)C=CC3C1C2 ISRJTGUYHVPAOR-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 229920006270 hydrocarbon resin Polymers 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 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
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000007645 offset printing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000001044 red dye Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、試料中の各成分の形状、大きさ、官能基の種
類、誘電率等の違いによる分配係数の差を利用して物質
の分離、定性、定量に用いられるｍＮクロマトグラフィ
ー用プレートおよびその製造方法に関するものである。Detailed Description of the Invention [Industrial Application Field] The present invention utilizes differences in distribution coefficients due to differences in shape, size, type of functional group, dielectric constant, etc. of each component in a sample. The present invention relates to an mN chromatography plate used for separation, qualitative, and quantitative determination, and a method for manufacturing the same.
従来から知られている薄層クロマトグラフィー用プレー
トは、ガラス板、プラスチックス板等の基板の上に、ア
ルミナ又はシリカゲル等の微粉末（数μｌｌ〜５０μ■
程度）からなる吸着剤を少量のバインダーと共に、アプ
リケーターで均一な厚さ（０，１〜０．３ｍ）に展着塗
布して作製されたものである。そして、この薄層クロマ
トグラフィー用プレートは、原点即ちスポット箇所に試
料を付着させ、展開槽中で溶媒を毛細管現象により展開
させ、分離することによって使用されている。Conventionally known plates for thin layer chromatography are made of fine powder such as alumina or silica gel (several microliters to 50 microliters) placed on a substrate such as a glass plate or a plastic plate.
It was prepared by spreading and applying an adsorbent consisting of 300 ml (about 100 ft) to a uniform thickness (0.1 to 0.3 m) with a small amount of binder using an applicator. This plate for thin layer chromatography is used by attaching a sample to the origin, ie, a spot, and then developing and separating the solvent in a developing tank by capillary action.
このようにして行われる薄層クロマトグラフィーは、利
用のし易さ、コスト等の諸点において、従来から用いら
れている他の分離分析法に比し優れており、各種分野で
採用されている。Thin layer chromatography performed in this manner is superior to other conventionally used separation and analysis methods in terms of ease of use, cost, etc., and has been adopted in various fields.
しかし、前記した従来の薄層クロマトグラフィー用プレ
ートには、次のような問題点があった。However, the conventional thin layer chromatography plate described above has the following problems.
吸着剤を基板に固定する為のバインダーの比率が多いと
分離能や展開能が悪くなるので、バインダーの比率は吸
着剤に対して数％以内に押さえられている。その為、吸
着剤の基板に対する密着性が悪く、表面が擦れると吸着
剤がボロボロと取れるという保管上の問題点があった。If the ratio of the binder for fixing the adsorbent to the substrate is too large, the separation ability and development performance will deteriorate, so the ratio of the binder to the adsorbent is kept within a few percent. Therefore, the adhesiveness of the adsorbent to the substrate is poor, and when the surface is rubbed, the adsorbent comes off in pieces, which is a storage problem.
また、吸着剤の粉末粒子間の毛細管現象を利用するもの
であるため、展開液の展開できる孔サイズが限られた範
囲のものになり、例えば樹脂、オリゴマー等の分子量が
大きく、嵩が高いものを展開するには不適当であるとい
う問題点があった。In addition, since it utilizes the capillary phenomenon between powder particles of the adsorbent, the pore size that can be developed by the developing solution is limited. The problem was that it was unsuitable for development.
さらに、製造方法においては、アルミナ又はシリカゲル
等の焼成工程、微粉砕工程２分級工程。Furthermore, the manufacturing method includes a firing step for alumina or silica gel, a pulverization step, and a classification step.
展着塗布工程等の諸工程を経て吸着剤層が形成されるの
で、非常に煩雑であると共にコスト高になるという問題
点があった。Since the adsorbent layer is formed through various processes such as a spread coating process, there are problems in that it is very complicated and increases the cost.
本発明者は、前記した従来技術においては種々の課題が
存するので、これを解決すべく研究した結果、従来技術
とは全く異なる構造の本発明に係る薄層クロマトグラフ
ィー用プレート及びその製造方法を完成するに至ったの
である。The present inventor has conducted research to solve various problems in the prior art described above, and has developed a plate for thin layer chromatography according to the present invention having a structure completely different from that of the prior art, and a method for manufacturing the same. It was completed.
即ち、本発明に係る薄層クロマトグラフィー用プレート
は、基板ｌの表面に該基板に沿った孔２又は溝３を有す
る金属酸化物皮膜４が形成され、前記した孔２又は溝３
の内部が外気と通じていることを特徴とするものである
。That is, in the plate for thin layer chromatography according to the present invention, a metal oxide film 4 having holes 2 or grooves 3 along the substrate is formed on the surface of a substrate l, and the holes 2 or grooves 3 described above are formed on the surface of the substrate l.
It is characterized by its interior communicating with the outside air.
次に、本発明を図面に基づいて詳細に説明する。Next, the present invention will be explained in detail based on the drawings.
本発明において使用する基板としては、アクリル、ポリ
エステル、ポリイミド、ポリフェニレンサルファイド、
ポリアミドイミド、ポリエーテルエーテルケトンケトン
５ポリアミド、液晶ポリマーなどのプラスチックス、ガ
ラス繊維、炭素繊維。Substrates used in the present invention include acrylic, polyester, polyimide, polyphenylene sulfide,
Plastics such as polyamideimide, polyetheretherketoneketone 5 polyamide, liquid crystal polymer, glass fiber, carbon fiber.
有機繊維などで強化したプラスチックス、ソーダガラス
、ホウケイ酸ソーダガラス、ホウケイ酸バリウムガラス
、石英ガラスなどのガラス、シリカ。Plastics reinforced with organic fibers, glasses such as soda glass, soda borosilicate glass, barium borosilicate glass, quartz glass, and silica.
アルミナ、チタニア、ジルコニアなどのセラミックス、
チタン、アルミニウム、ニッケル、鉄、銅。Ceramics such as alumina, titania, and zirconia,
Titanium, aluminum, nickel, iron, copper.
銀、金またはこれらの合金などの金属、タイル、琺瑯、
陶磁器などが用いられる。特に透明性が必要な場合は、
透明なガラスやプラスチックスが用いられる。なお、基
板の形状としては、平面体、曲面体を問わずどのような
ものでもよい。Metals such as silver, gold or their alloys, tiles, enamel,
Ceramics etc. are used. Especially when you need transparency.
Transparent glass or plastics are used. Note that the substrate may have any shape, regardless of whether it is a flat body or a curved body.
基板ｌ上に形成される金属酸化物皮膜４を構成する金属
元素としては、アルミニウム、チタニウム、ゲイ素、ジ
ルコニウム、インジウム、スズ２亜鉛、ゲルマニウム、
イツトリウム、スカンジウム、ガリウム、ニオブ、タン
タル、ハフニウム。Metal elements constituting the metal oxide film 4 formed on the substrate l include aluminum, titanium, silicon, zirconium, indium, tin dizinc, germanium,
Yztrium, scandium, gallium, niobium, tantalum, hafnium.
ニッケル、コバルト、クロム、鉄、マンガン、マグネシ
ウム、希土類元素などを挙げることができる。これらの
内、アルミニウム、チタニウム、ケイ素、マグネシウム
、ジルコニウムを用いると、多孔性、透明性、造膜性の
点において特に優れている。前記した従来技術において
は、アルミナ又はシリカゲル等の微粉末からなる吸着剤
が白色であるため反射光しか利用できないが、本発明で
は金属酸化物皮膜４を透明にすることも可能であり、こ
の場合には透過光を利用し、ランバート・ベールの法則
を適用して、分離したものの濃度を正確に測定すること
ができる。Examples include nickel, cobalt, chromium, iron, manganese, magnesium, and rare earth elements. Among these, aluminum, titanium, silicon, magnesium, and zirconium are particularly excellent in terms of porosity, transparency, and film-forming properties. In the conventional technology described above, only reflected light can be used because the adsorbent made of fine powder such as alumina or silica gel is white, but in the present invention, it is also possible to make the metal oxide film 4 transparent, and in this case. By using transmitted light and applying the Lambert-Beer law, it is possible to accurately measure the concentration of separated substances.
前記した金属元素を混合した金属酸化物皮膜を用いると
、二以上の金属元素の持つ特性を生がした複合膜を得る
ことができる。また、金属酸化物皮膜４を異なる二以上
の積層物とすれば、試料に合わせた特性を有するものを
得ることができる。By using a metal oxide film containing a mixture of the metal elements described above, it is possible to obtain a composite film that takes advantage of the characteristics of two or more metal elements. Moreover, if the metal oxide film 4 is made of a laminate of two or more different layers, it is possible to obtain a film having characteristics suited to the sample.
なお、金属酸化物皮Ｍ４が透明であると、ランバート・
ベールの法則を適用できるので、分離したものの濃度を
正確に測定することができるという利点がある。In addition, if the metal oxide skin M4 is transparent, the Lambertian
Since Beer's law can be applied, it has the advantage that the concentration of separated substances can be measured accurately.
金属酸化物皮膜を形成する方法としては、基板に、金属
アルコキシド又は金属塩の加水分解物。As a method for forming a metal oxide film, a hydrolyzate of a metal alkoxide or metal salt is applied to the substrate.
金属酸化物の溶解物又はコロイド物等の金属酸化物の水
和物の分散液（ゾルとか金属酸化物系ポリマー溶液とも
呼ばれている。）、金属アルコキシド等の金属化合物を
スプレー法、スピナー法、デイピング法、リバースコー
ター、ロールコータ−等のコーター法、グラビア、スク
リーン等の印刷法等で塗布した後、焼成する方法が代表
的なものである。その他、金属、金属アルコキシド、金
属酸化物をＰＩＤ法（蒸着、゛スパッタリング、イオン
ブレーティング）、ＣＶＤ法により基板上に設置し、必
要に応じて酸化、焼成等をおこなう方法等がある。金属
酸化物の水和物の分散液を用いる方法は、膜厚を厚くす
ることが容易であるので優れている。A dispersion of a metal oxide hydrate such as a dissolved metal oxide or a colloid (also called a sol or a metal oxide polymer solution), a metal compound such as a metal alkoxide, and a spray method or spinner method Typical methods include coating by a dipping method, a coater method such as a reverse coater or a roll coater, or a printing method such as gravure or screen, followed by baking. Other methods include placing a metal, metal alkoxide, or metal oxide on a substrate by a PID method (vapor deposition, sputtering, ion blating) or CVD method, and performing oxidation, firing, etc. as necessary. The method using a dispersion of metal oxide hydrate is advantageous because it is easy to increase the film thickness.
前記した従来法によれば、吸着剤層がアルミナ又はシリ
カゲル等の微粉末の積層によって構成されているので、
その表面を平滑にすることは不可能でちるが、本発明に
おいては、吸着剤層を構成する金属酸化物皮膜層４を上
記方法により形成することができるので、その表面が平
滑なものをも得ることができる。このように金属酸化物
皮膜４の表面を平滑なものとすれば、乱反射が生じない
ので、分離したものの濃度を正確に測定することができ
る。According to the conventional method described above, since the adsorbent layer is composed of a laminated layer of fine powder such as alumina or silica gel,
Although it is impossible to make the surface smooth, in the present invention, since the metal oxide film layer 4 constituting the adsorbent layer can be formed by the above method, it is possible to make the surface smooth. Obtainable. If the surface of the metal oxide film 4 is made smooth in this way, diffuse reflection will not occur, so that the concentration of the separated material can be accurately measured.
次に、孔２又は溝３を形成する方法について説明する。Next, a method for forming the holes 2 or grooves 3 will be explained.
概括すれば、基板１上に図柄形成物６を設けた後、その
上に前記した金属酸化物皮膜４を形成し、図柄形成物６
を除去することにより孔２又は溝３を形成すればよい、
前記した図柄形成物６の形状は、孔２又は溝３の形状に
相当する形状とされる。このような形状としては、例え
ば、直線２曲線、波線１円弧状、渦巻き状、あるいはこ
れらが縦横に重なった格子状など使用する目的に応じて
設計するとよい。また、その幅、長さ、高さなども特に
限定されないが、孔２又は溝３の高さが０．１〜１０μ
■９幅が１〜５０００μ謹のものが、展開したスポット
の読み取りの容易さ等がら適している。特に樹脂やオリ
ゴマー等の分子量、嵩の高い物を展開させる場合には、
孔２又は溝３の幅又は高さを大きくした方がよい、孔２
又は溝３の幅と孔２又は溝３間の距離との比が１／２以
下の方が作業性や膜強度の安定性等から適している。Generally speaking, after the pattern formation 6 is provided on the substrate 1, the metal oxide film 4 described above is formed thereon, and the pattern formation 6 is formed on the substrate 1.
The holes 2 or grooves 3 may be formed by removing the
The shape of the pattern formation 6 described above corresponds to the shape of the hole 2 or the groove 3. Such a shape may be designed depending on the purpose of use, for example, two straight lines, one curved line, one wavy line, an arc shape, a spiral shape, or a lattice shape in which these shapes are overlapped vertically and horizontally. Further, the width, length, height, etc. are not particularly limited, but the height of the hole 2 or groove 3 is 0.1 to 10 μm.
(2) A width of 1 to 5000 μm is suitable for ease of reading the developed spot. Especially when developing materials with high molecular weight and bulk such as resins and oligomers,
Hole 2 where it is better to increase the width or height of hole 2 or groove 3
Alternatively, it is preferable that the ratio of the width of the grooves 3 to the distance between the holes 2 or the grooves 3 is 1/2 or less in terms of workability and stability of membrane strength.
図柄形成物６を構成する化合物としては、熱、光。Compounds constituting the pattern formation 6 include heat and light.
電子線、酵素、酸、アルカリ等で分解する化合物（例え
ば、アクリル系樹脂、酢酸ビニル系樹脂。Compounds that are decomposed by electron beams, enzymes, acids, alkalis, etc. (e.g. acrylic resins, vinyl acetate resins).
０−キノンジアジドノボラック系樹脂、酢酸セルロース
系樹脂、セルロース系樹脂等がある。）、溶剤、酸、ア
ルカリに溶解する化合物（例えば、アクリル系樹脂、酢
酸ビニルとエチレンの共重合体系樹脂、塩化ビニル酢酸
ビニル共重合体系樹脂。Examples include 0-quinonediazide novolac resin, cellulose acetate resin, and cellulose resin. ), compounds soluble in solvents, acids, and alkalis (e.g., acrylic resins, vinyl acetate and ethylene copolymer resins, vinyl chloride vinyl acetate copolymer resins).
アクリル酸系樹脂、ポリエチレングリコール系樹脂、ポ
リエチレンオキサイド系樹脂等がある。）等がある０図
柄を設ける方法としては、オフセット印刷、スクリーン
印刷、グラビア印刷、インクジェット印刷などの印刷法
、スライド転写法、熱転写法などの転写法、レジスト法
（可視光や紫外光、電子線用のレジストを塗布し、露光
・現像して不要部を除去し、パターン化する方法）、刷
毛刷り法、スプレー法などがあるが、パターン精度、再
現性の点からは印刷法、転写法およびレジスト法がよい
、印刷法、転写法、レジスト法などを用いる際に、イン
キ中に熱、光、電子線、酵素、溶剤、酸、アルカリに分
解又は溶解するような塩基性染料、酸性染料、分散染料
、油溶性染料等を加えておくと図柄形成物６の確認が容
易となる。図柄形成物６として成形物を用いてもよく、
基板ｌ上に、天然繊維、合成繊維、プラスチックスなど
の成形物を必要な図柄に自然静置あるいは接着剤などを
用いて！！置すればよい。Examples include acrylic acid resins, polyethylene glycol resins, and polyethylene oxide resins. ), printing methods such as offset printing, screen printing, gravure printing, inkjet printing, transfer methods such as slide transfer method and thermal transfer method, resist method (visible light, ultraviolet light, electron beam There are several methods, such as applying a resist, exposing and developing it to remove unnecessary parts, and creating a pattern), brush printing, spraying, etc. However, from the viewpoint of pattern accuracy and reproducibility, printing, transfer, and When using a printing method, a transfer method, a resist method, etc., for which the resist method is better, basic dyes, acidic dyes, etc. that are decomposed or dissolved in heat, light, electron beams, enzymes, solvents, acids, and alkalis are used. If disperse dyes, oil-soluble dyes, etc. are added, the design formations 6 can be easily confirmed. A molded object may be used as the pattern formed object 6,
On the substrate l, molded materials such as natural fibers, synthetic fibers, plastics, etc. can be left in the desired pattern naturally or using adhesives! ! Just put it there.
前記した図柄形成物６は、金属酸化物皮膜４で覆われた
後、熱、光、電子線、酵素、溶剤、酸。After the pattern formation 6 is covered with the metal oxide film 4, it is exposed to heat, light, electron beams, enzymes, solvents, and acids.
アルカリで分解又は溶解して除去される。・なお、この
発明において孔２は、基板１と金属酸化物皮膜４との界
面に形成されるか、または、金属酸化物皮膜４中に形成
される。そして、この孔２は基板ｌに沿って形成され、
連続している。It is removed by decomposition or dissolution with alkali. - In this invention, the holes 2 are formed at the interface between the substrate 1 and the metal oxide film 4, or in the metal oxide film 4. Then, this hole 2 is formed along the substrate l,
Continuous.
溝３の場合も、基板１に沿って形成され、連続している
。この孔２又は溝３に発色性試薬を吸着させておくと、
物質の定性及び濃度の定量ができるという利点がある。The groove 3 is also formed along the substrate 1 and is continuous. If a coloring reagent is adsorbed in this hole 2 or groove 3,
It has the advantage of being able to qualitatively quantify substances and quantify concentrations.
ところで、溝３の場合は、その全長にわたって外気と通
じているが、孔２の場合はその内部が外気と少なくとも
三箇所において通じている。この孔２の内部が外気と通
じている箇所は、孔２の端面であってもよく、また、孔
２の端面と端面との間に形成された割れ目５でもよい０
割れ目５は、金属酸化物皮膜４０表面から孔２の内部に
至っている必要がある。この割れ目５の作製方法として
は、例えば図柄形成物６をガス化させて、これを金属酸
化物皮膜４中に急激に飛散させて割れ目５を住しさせた
り、金属酸化物皮Ｍ４の表面を金属刃物等で傷をつけた
りする方法等がある０割れ目５を設ける方法については
前記した通りであるが、図柄形成物６をガス化させて割
れ目５を設ける場合１．原点に割れ目５が生じると円状
の原点スポットが得られないという問題点が起こる。そ
こで、原点において割れ目５が生じないようにするため
には、次のようにすればよい、即ち、前記したと同様に
、孔２の形状に相当し且つ焼成により割れ目５を住しさ
せる図柄形成物６を基板１の表面に設けた後、金属酸化
物皮膜形成物を設け、次いで原点の図柄形成物６を除去
し、焼成すればよい。By the way, in the case of the groove 3, the entire length thereof communicates with the outside air, but in the case of the hole 2, the inside thereof communicates with the outside air at at least three points. The location where the inside of the hole 2 communicates with the outside air may be the end surface of the hole 2, or may be the crack 5 formed between the end surfaces of the hole 2.
The crack 5 must extend from the surface of the metal oxide film 40 to the inside of the hole 2 . The cracks 5 can be created by, for example, gasifying the pattern forming material 6 and rapidly scattering it into the metal oxide film 4 to form the cracks 5, or by changing the surface of the metal oxide film M4. The method of creating the cracks 5, which includes making scratches with a metal knife, etc., is as described above, but when creating the cracks 5 by gasifying the pattern forming material 6, 1. If a crack 5 occurs at the origin, a problem arises in that a circular origin spot cannot be obtained. Therefore, in order to prevent the cracks 5 from occurring at the origin, the following steps should be taken: In the same way as described above, form a pattern that corresponds to the shape of the hole 2 and that allows the cracks 5 to be formed by firing. After the object 6 is provided on the surface of the substrate 1, a metal oxide film forming object is provided, and then the pattern forming object 6 at the origin is removed and firing is performed.
このようにすることによって、基板ｌの表面に図柄形成
物６の形状に相当する孔２を有し、且つ原点以外の箇所
に金属酸化物皮膜４の表面から孔２に至る割れ目５を有
する金属酸化物皮膜４を形成した薄層クロマトグラフィ
ー用プレートを製造することができる。なお、金属酸化
物皮膜形成物としては、前記した金属酸化物の水和物の
分散液を原料とするもの、金属蒸着によるもの等がある
。By doing so, a metal having a hole 2 corresponding to the shape of the pattern formation 6 on the surface of the substrate l and having a crack 5 extending from the surface of the metal oxide film 4 to the hole 2 at a location other than the origin. A plate for thin layer chromatography on which the oxide film 4 is formed can be manufactured. Note that metal oxide film-formed products include those made from the above-mentioned dispersion of hydrates of metal oxides, those made by metal vapor deposition, and the like.
前記した割れ目５を設けておくと、発色試薬を噴霧した
際に、試薬が割れ目５から浸入して試料と反応するので
、容易に発色させることができる。If the cracks 5 described above are provided, when the coloring reagent is sprayed, the reagent will enter through the cracks 5 and react with the sample, making it easy to develop color.
また、試料と金属酸化物との接触面積が増えるので、反
応容量が増える。さらに、展開時間が短縮できるという
効果が得られる。一方、スポット誤差が生じないように
するためには、割れ目５を設けない方がよい。Furthermore, since the contact area between the sample and the metal oxide increases, the reaction capacity increases. Furthermore, the effect that the development time can be shortened can be obtained. On the other hand, in order to prevent spot errors from occurring, it is better not to provide the cracks 5.
次に、本発明に係る薄層クロマトグラフィー用プレート
の使用方法について説明する。Next, a method of using the thin layer chromatography plate according to the present invention will be explained.
試料を適当な溶媒に溶解した後、本発明に係る薄層クロ
マトグラフィー用プレートの下端から１５〜２０■程度
の位置の原点にスポットし、乾燥する。After dissolving the sample in a suitable solvent, it is spotted at the origin at a position approximately 15 to 20 cm from the bottom of the plate for thin layer chromatography according to the present invention, and dried.
次に、分離するのに最も適した誘電率を有する展開溶媒
を入れた展開槽に原点側を下にして適当な角度を持たせ
て立てる。展開溶媒は毛細管作用により孔２又は溝３を
浸透する。一定距離展開した後に薄層クロマトグラフィ
ー用プレートを取り出し、乾燥し、次いで各種方法によ
り検出し、記録する。Next, stand the sample at an appropriate angle with the origin side facing down in a developing tank containing a developing solvent with the most suitable dielectric constant for separation. The developing solvent permeates through the holes 2 or grooves 3 by capillary action. After developing for a certain distance, the thin layer chromatography plate is taken out, dried, and then detected and recorded by various methods.
試料が無色の場合は、発色試薬、例えば、濃硫酸、過マ
ンガン酸カリと硫酸の混合液２重クロム酸ナトリウムと
硫酸の混合液、ヨウ素、塩化アンチモン等の無機試薬、
また、ニンヒドリンブロモクレゾールグリーン、２．４
ジニトロフエニルヒドラジン、ドラジェンドルフ試薬等
の有機試薬を用いて発色させた後、一方、試料が有色で
ある場合はそのまま、−船釣な薄層クロマトグラフィー
のＲｆ値比較法により定性を行い、色濃度を紫外・可視
分光光度計等で測定することにより定量を行う。If the sample is colorless, use a coloring reagent such as concentrated sulfuric acid, a mixture of potassium permanganate and sulfuric acid, a mixture of sodium dichromate and sulfuric acid, iodine, an inorganic reagent such as antimony chloride,
Also, ninhydrin bromocresol green, 2.4
After developing a color using an organic reagent such as dinitrophenylhydrazine or Dragendorff's reagent, if the sample is colored, it is qualitatively determined using the Rf value comparison method of thin layer chromatography. Quantification is performed by measuring color density using an ultraviolet/visible spectrophotometer.
また、前記したＲｆ値法以外に、展開して分離したスポ
ットをかき集めて溶媒で抽出して遠赤外線分光光度計を
用いて定性することもできる。この遠赤外線分光光度計
を用いた透過定性法では、反射定性法に比べて測定感度
が極端に高いので、低濃度でも定性が可能である。特に
本発明の透明タイプを用いた場合には、スポット部をか
き集める必要がなく、展開した基板上のスポット部のみ
に遠赤外線を透過させることにより容易に定性ができる
。In addition to the above-mentioned Rf value method, it is also possible to collect the developed and separated spots, extract them with a solvent, and qualitatively analyze them using a far-infrared spectrophotometer. In the transmission qualitative method using this far-infrared spectrophotometer, the measurement sensitivity is extremely high compared to the reflection qualitative method, so qualitative determination is possible even at low concentrations. In particular, when the transparent type of the present invention is used, there is no need to collect the spot portions, and qualitative determination can be easily performed by transmitting far infrared rays only through the spot portions on the developed substrate.
試料は、それぞれ形状、大きさ、官能基の種類、誘電率
の違いによって、金属酸化物に対する親和性が異なるの
でこの特性を利用して金属酸化物皮膜中の孔又は溝の中
を分離しようとする試料が展開液と一緒に展開される際
、その親和性の違いにより分離される。Samples have different affinities for metal oxides depending on their shape, size, type of functional group, and dielectric constant, so we tried to utilize these characteristics to separate the inside of the pores or grooves in the metal oxide film. When a sample is developed with a developing solution, it is separated due to differences in affinity.
実施例１
透明ガラス基板の上に、アクリル樹脂より成るスクリー
ンインキを用いて、直線状図柄をスクリーン印刷した後
、アルミナゾルをスプレーコーティングした０次に、５
００°Ｃ３時間焼成して、表面に割れ目のある孔及び溝
を有する薄層クロマトグラフィー用プレートを得た。Example 1 A linear pattern was screen-printed on a transparent glass substrate using screen ink made of acrylic resin, and then alumina sol was spray-coated.
By baking at 00°C for 3 hours, a plate for thin layer chromatography having holes and grooves with cracks on the surface was obtained.
実験例１
実施例１で得た薄層クロマトグラフィー用プレート（以
下、本発明品ｌという。）と、アルミナ微粉末からなる
吸着剤をバインダーと共にガラス板に展着塗布した従来
の薄層クロマトグラフィー用プレート（以下、従来品１
という、）との特性について比較実験を行った。Experimental Example 1 Conventional thin layer chromatography using the plate for thin layer chromatography obtained in Example 1 (hereinafter referred to as Invention Product 1) and an adsorbent made of fine alumina powder spread and coated on a glass plate together with a binder. plate (hereinafter, conventional product 1)
We conducted a comparative experiment on the characteristics of
〈耐摩擦性〉
本発明重工及び従来品１を指で軽く擦った０本発明品１
ではアルミニウム酸化皮膜が取れることはなかったが、
従来品１では表面のアルミナ微粉末が取れた。<Abrasion resistance> Invention product 1 by lightly rubbing the invention heavy industry and conventional product 1 with fingers
However, the aluminum oxide film could not be removed.
With conventional product 1, fine alumina powder on the surface could be removed.
〈分離性能〉 アルミナに対して吸着性のある赤色染料（Ｃ，Ｉ。<Separation performance> Red dyes (C, I) adsorbent to alumina.
デイスパースレッド６０）と吸着性のない青色染料（Ｃ
，！、ソルベントブルー９７）を混合した溶液を、それ
ぞれの薄層クロマトグラフィー用プレートにスポットし
て、トルエンと酢酸エチルがｌ：１の展開液に浸けて展
開したところ、両方とも同じように分離した。Disperse red 60) and non-adsorbent blue dye (C
，! , Solvent Blue 97) was spotted on each plate for thin layer chromatography, and when the plates were immersed in a developing solution of 1:1 of toluene and ethyl acetate and developed, both plates were separated in the same way.
く染料濃度測定〉
本発明品１は、アルミナ皮膜が透明であるので、ランバ
ート・ベールの法則が適用でき、分光光度計により混合
液中の染料濃度を正確に測定できた、しかし、従来品１
は、反射濃度でしかも表面に凹凸があるので、染料濃度
の正確な測定は、不可能であった。Measurement of Dye Concentration> Since the alumina film of Inventive Product 1 is transparent, the Beer-Lambert law can be applied, and the dye concentration in the mixture can be accurately measured using a spectrophotometer. However, Conventional Product 1
Because of the reflection density and the unevenness of the surface, it was impossible to accurately measure the dye concentration.
実施例２
アクリル樹脂と側鎖を有する炭化水素系樹脂から成るイ
ンキを用いて作成した転写箔によりポリエステル基板上
に直線柄を転写した後、アルミニウムアルコキシド及び
ケイ酸アルコキシドの加水分解物（アルミニウム：ケイ
素＝１：４）を用いてアルミナ−シリカ複合酸化物皮膜
を形成した。Example 2 After a linear pattern was transferred onto a polyester substrate using a transfer foil made using an ink made of an acrylic resin and a hydrocarbon resin having side chains, a hydrolyzate of aluminum alkoxide and silicate alkoxide (aluminum:silicon) was transferred. = 1:4) to form an alumina-silica composite oxide film.
次に、電子線を照射して樹脂を分解し、１８０℃６０分
加熱した後、アセトン溶液中で超音波洗浄した。Next, the resin was decomposed by irradiation with an electron beam, heated at 180° C. for 60 minutes, and then subjected to ultrasonic cleaning in an acetone solution.
その結果、孔を有する薄層クロマトグラフィー用プレー
トを得た。両端部及び原点において、孔と直角な方向に
カッターナイフにより切れ目を入れて割れ目とした。As a result, a plate for thin layer chromatography having holes was obtained. At both ends and at the origin, a cut was made with a cutter knife in a direction perpendicular to the hole to form a crack.
実験例２
原点に紫色染料（Ｃ，１，デイスパースバイオレット６
）と青色染料（Ｃ，１，デイスパースブルー３５）から
成る混合液をスポットした後、トルエン液で展開させた
ところ、紫色染料（Ｃ，１，デイスパースバイオレット
６）が原点から離れたところ、青色染料（Ｃ，１，デイ
スパースブルー３５）が原点に近いところに展開された
。 Ｒｆ値でその定性及び分光光度計で、６量の定量を
行った。Experimental Example 2 Purple dye (C, 1, Disperse Violet 6) at the origin
) and a blue dye (C, 1, Disperse Blue 35) was spotted and developed with toluene solution. When the purple dye (C, 1, Disperse Violet 6) moved away from the origin, A blue dye (C,1, Disperse Blue 35) was developed close to the origin. Six quantities were determined qualitatively by Rf value and quantitatively by spectrophotometer.
実施例３
石英ガラス基板にアルミナ水和物の分散液を塗布した後
、２５０°Ｃ３０分乾燥した０次に、その上にアクリル
樹脂から成るスクリーンインキを用いて直線柄を設けた
後、アルミナ−マグネシア（アルミニウム：マグネシウ
ム−９：１）の水和物の分散液を塗布した後、５００℃
８時間焼成し、割れ目のある孔を有する薄層クロマトグ
ラフィー用プレートを得た。Example 3 After applying a dispersion of alumina hydrate to a quartz glass substrate, it was dried at 250°C for 30 minutes, and then a linear pattern was provided thereon using screen ink made of acrylic resin. After applying a dispersion of magnesia (aluminum:magnesium-9:1) hydrate,
After baking for 8 hours, a plate for thin layer chromatography having cracked pores was obtained.
実験例３
く分離性能〉
実施例３で得た薄層クロマトグラフィー用プレート（以
下、本発明品２という。）及び従来品１をそれぞれ二枚
用意し、炭化水素系オリゴマーとアクリル系樹脂とから
成る混合液をスポットし、その隣に青色染料（Ｃ，１，
デイスパースブルー９７）の液をスポットした。トルエ
ンと酢酸エチルの比が７：３の展開液で展開した。展開
の終了点は青色染料が上端まで展開した時点とした。Experimental Example 3 Separation Performance> Two plates each of the thin layer chromatography plate obtained in Example 3 (hereinafter referred to as the present invention product 2) and the conventional product 1 were prepared, and a hydrocarbon oligomer and an acrylic resin were separated. A mixture of blue dye (C, 1,
A solution of Disperse Blue 97) was spotted. It was developed with a developing solution containing toluene and ethyl acetate in a ratio of 7:3. The end point of development was the time when the blue dye developed to the top.
く樹脂濃度測定〉
次に、本発明品２及び従来品１のそれぞれ一枚を、よう
素が飽和したビン中に一定時問いれて発色させて、試料
が分離した位置を確認したところ、本発明品２では分離
していたが、従来品ｌでは分離していなかった０本発明
品２については、さらに分光光度計で濃度を求めた。Measurement of Resin Concentration> Next, one sheet each of Inventive Product 2 and Conventional Product 1 was placed in a bottle saturated with iodine for a certain period of time to develop color, and the position where the sample was separated was confirmed. Invention product 2 was separated, but conventional product 1 was not separated. Regarding invention product 2, the concentration was further determined using a spectrophotometer.
本発明品２の残りの一枚を用いて、発色していない分離
した試料を、分光光度計で紫外域の吸収濃度を測定し、
その値からアクリル系樹脂の濃度を求めた。又遠赤外線
分光光度計で定性を行った。Using the remaining sheet of Invention Product 2, the absorption concentration in the ultraviolet region was measured using a spectrophotometer for the separated sample that did not develop color.
The concentration of the acrylic resin was determined from that value. Qualitative analysis was also performed using a far-infrared spectrophotometer.
実施例４
ガラス基板上に０−キノンジアジドノボラック系樹脂か
らなるレジストを用いて波線図柄を設け、その上にアル
ミニウムを蒸着した０次に、ガラス基板面側から紫外線
を照射して樹脂を分解した。Example 4 A wavy line pattern was provided on a glass substrate using a resist made of 0-quinonediazide novolac resin, and aluminum was vapor-deposited thereon.Then, the resin was decomposed by irradiating ultraviolet rays from the glass substrate surface side.
その後、オゾン酸性雰囲気中でアルミニウム膜を酸化し
てアルミナ皮膜にした０次いで、アセトン液中で超音波
洗浄して樹脂を除去して、孔を有する薄層クロマトグラ
フィー用プレートを得た９両端部において孔と直角な方
向にカッターナイフにより切れ目を入れて割れ目とした
。Thereafter, the aluminum film was oxidized to form an alumina film in an ozone acidic atmosphere.Next, the resin was removed by ultrasonic cleaning in an acetone solution to obtain a plate for thin layer chromatography having holes at both ends. A cut was made with a cutter knife in a direction perpendicular to the hole to form a crack.
実験例４
実施例４によって得た薄層クロマトグラフィー用プレー
トに、オレンジ染料（Ｃ，１，デイスパースオレンジ１
１）と青色染料（Ｃ，ｌデイスパースブルー３５）の混
合液をスポットしてメチルエチルチトン液で展開したと
ころ、オレンジ染料と青色染料は分離し、それぞれ分光
光度計で定量できた。Experimental Example 4 Orange dye (C,1, Disperse Orange 1) was applied to the plate for thin layer chromatography obtained in Example 4.
When a mixture of 1) and blue dye (C,l Disperse Blue 35) was spotted and developed with methyl ethyl titone solution, the orange dye and blue dye were separated and each could be quantified using a spectrophotometer.
本発明は以上の構成よりなるから、次の諸効果が奏され
る。Since the present invention has the above configuration, the following effects are achieved.
本発明に係る薄層クロマトグラフィー用プレートは、金
属酸化物皮膜が基板に固着しているので、表面強度が強
く、保管が容易である。Since the thin layer chromatography plate according to the present invention has a metal oxide film fixed to the substrate, it has strong surface strength and is easy to store.
また、孔又は溝の毛細管現象を利用するものであるため
、展開液の展開できる孔サイズを大きくすることも可能
であり、例えば樹脂、オリゴマー等の分子量が大きく、
嵩が大きい°ものでも適用が可能である。In addition, since it utilizes the capillary phenomenon of holes or grooves, it is possible to increase the size of the pores that can be developed by the developing solution.For example, when the molecular weight of resin, oligomer, etc. is large,
It can also be applied to items with large bulk.
さらに、本発明に係る薄層クロマトグラフィー用プレー
トの製造方法は、基板上に図柄形成物を設けた後金属酸
化物皮膜を形成し、次いで図柄形成物を除去するだけで
あるから、薄層クロマトグラフィー用プレートを簡単に
且つ低コストで得ることができる。Furthermore, the method for manufacturing a plate for thin layer chromatography according to the present invention simply involves forming a pattern formation on a substrate, forming a metal oxide film, and then removing the pattern formation. A graphics plate can be obtained easily and at low cost.
第１図及び第２図は、本発明に係る薄層クロマトグラフ
ィー用プレートの斜視説明図を示す。
図中 １・−・基板、２−孔、３−溝、４−金属酸化物
皮膜、５・・割れ目。FIGS. 1 and 2 are perspective explanatory views of a plate for thin layer chromatography according to the present invention. In the figure: 1--Substrate, 2--hole, 3--groove, 4--metal oxide film, 5--crack.
Claims (1)
又は溝（３）を有する金属酸化物皮膜（４）が形成され
、前記した孔（２）又は溝（３）の内部が外気と通じて
いることを特徴とする薄層クロマトグラフィー用プレー
ト。 ２、孔（２）の内部が外気と少なくとも２箇所において
通じていることを特徴とする特許請求の範囲第１項に記
載の薄層クロマトグラフィー用プレート。 ３、孔（２）の内部が外気と通じている少なくとも一箇
所が、孔（２）の端面である特許請求の範囲第２項に記
載の薄層クロマトグラフィー用プレート。 ４、孔（２）の内部が外気と通じている少なくとも一箇
所が、金属酸化物皮膜（４）の表面から孔（２）の内部
に至る割れ目（４）である特許請求の範囲第２項又は第
３項に記載の薄層クロマトグラフィー用プレート。 ５、金属酸化物皮膜（４）が、金属酸化物の水和物の分
散液を原料として形成されたものである特許請求の範囲
第１項〜第４項の何れかに記載の薄層クロマトグラフィ
ー用プレート。 ６、金属酸化物皮膜（４）が、アルミニウム、ケイ素、
チタニウム、マグネシウム、ジルコニウムから選ばれる
元素の酸化物皮膜である特許請求の範囲第１項〜第５項
の何れかに記載の薄層クロマトグラフィー用プレート。 ７、金属酸化物皮膜（４）が、アルミニウム、ケイ素、
チタニウム、マグネシウム、ジルコニウムの少なくとも
二以上の元素の複合酸化物皮膜である特許請求の範囲第
１項〜第５項の何れかに記載の薄層クロマトグラフィー
用プレート。 ８、金属酸化物皮膜（４）が、透明である特許請求の範
囲第１項〜第７項の何れかに記載の薄層クロマトグラフ
ィー用プレート。 ９、孔（２）又は溝（３）が、発色性試薬を吸着したも
のである特許請求の範囲第１項〜第８項の何れかに記載
の薄層クロマトグラフィー用プレート。 １０、孔（２）又は溝（３）の形状に相当する図柄形成
物（６）を基板（１）の表面に設けた後、金属酸化物の
水和物の分散液を塗布し、焼成することにより、基板（
１）の表面に図柄形成物（６）の形状に相当する孔（２
）又は溝（３）を有する金属酸化物皮膜（４）を形成す
ることを特徴とする特許請求の範囲第１項〜第９項の何
れかに記載の薄層クロマトグラフィー用プレートの製造
方法。 １１、孔（２）又は溝（３）の形状に相当し且つ焼成に
より割れ目（５）を生じさせる図柄形成物（６）を基板
（１）の表面に設けた後、金属酸化物皮膜形成物を設け
、乾燥し、次いで原点の図柄形成物（６）を除去し、焼
成することにより、基板（１）の表面に図柄形成物（６
）の形状に相当する孔（２）又は溝（３）を有し、且つ
原点以外の箇所に金属酸化物皮膜（４）の表面から孔（
２）又は溝（３）に至る割れ目（５）を有する金属酸化
物皮膜（４）を形成することを特徴とする特許請求の範
囲第４項に記載の薄層クロマトグラフィー用プレートの
製造方法。[Claims] 1. A hole (2) on the surface of the substrate (1) along the substrate (1)
Or a plate for thin layer chromatography, characterized in that a metal oxide film (4) having grooves (3) is formed, and the insides of the holes (2) or grooves (3) are communicated with the outside air. 2. The plate for thin layer chromatography according to claim 1, wherein the inside of the hole (2) communicates with the outside air at at least two places. 3. The plate for thin layer chromatography according to claim 2, wherein at least one location through which the inside of the hole (2) communicates with the outside air is an end surface of the hole (2). 4. Claim 2, wherein at least one point where the inside of the hole (2) communicates with the outside air is a crack (4) extending from the surface of the metal oxide film (4) to the inside of the hole (2). Or the plate for thin layer chromatography according to item 3. 5. The thin layer chromatograph according to any one of claims 1 to 4, wherein the metal oxide film (4) is formed using a dispersion of metal oxide hydrate as a raw material. Graffiti plate. 6. The metal oxide film (4) is aluminum, silicon,
The plate for thin layer chromatography according to any one of claims 1 to 5, which is an oxide film of an element selected from titanium, magnesium, and zirconium. 7. The metal oxide film (4) is aluminum, silicon,
The plate for thin layer chromatography according to any one of claims 1 to 5, which is a composite oxide film of at least two or more elements of titanium, magnesium, and zirconium. 8. The plate for thin layer chromatography according to any one of claims 1 to 7, wherein the metal oxide film (4) is transparent. 9. The plate for thin layer chromatography according to any one of claims 1 to 8, wherein the holes (2) or grooves (3) have adsorbed a coloring reagent. 10. After providing a pattern formation (6) corresponding to the shape of the hole (2) or groove (3) on the surface of the substrate (1), a dispersion of metal oxide hydrate is applied and fired. By this, the substrate (
A hole (2) corresponding to the shape of the pattern formation (6) is formed on the surface of (1).
) or grooves (3), the method for producing a plate for thin layer chromatography according to any one of claims 1 to 9, characterized in that a metal oxide film (4) having grooves (3) is formed. 11. After providing on the surface of the substrate (1) a pattern-forming material (6) that corresponds to the shape of the hole (2) or groove (3) and that produces cracks (5) by firing, a metal oxide film-formed material is formed. The pattern formation material (6) is provided on the surface of the substrate (1) by drying, removing the pattern formation material (6) at the origin, and firing.
), and has holes (2) or grooves (3) corresponding to the shape of the metal oxide film (4) at a location other than the origin.
5. The method for producing a plate for thin layer chromatography according to claim 4, which comprises forming a metal oxide film (4) having cracks (5) extending to grooves (2) or grooves (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1305580A JPH03165260A (en) | 1989-11-22 | 1989-11-22 | Plate for thin-layer chromatography and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1305580A JPH03165260A (en) | 1989-11-22 | 1989-11-22 | Plate for thin-layer chromatography and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03165260A true JPH03165260A (en) | 1991-07-17 |
Family
ID=17946856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1305580A Pending JPH03165260A (en) | 1989-11-22 | 1989-11-22 | Plate for thin-layer chromatography and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03165260A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003530571A (en) * | 2000-04-07 | 2003-10-14 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフトング | Monolithic adsorbent with fiber reinforced plastic coating |
| JP2007198916A (en) * | 2006-01-26 | 2007-08-09 | Dainippon Printing Co Ltd | Defect detection method of transparent gas barrier film |
| CN102707012A (en) * | 2012-05-11 | 2012-10-03 | 北京大学 | Narrow band thin-layer chromatographic sheet and preparation method thereof |
-
1989
- 1989-11-22 JP JP1305580A patent/JPH03165260A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003530571A (en) * | 2000-04-07 | 2003-10-14 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフトング | Monolithic adsorbent with fiber reinforced plastic coating |
| JP2007198916A (en) * | 2006-01-26 | 2007-08-09 | Dainippon Printing Co Ltd | Defect detection method of transparent gas barrier film |
| JP4570049B2 (en) * | 2006-01-26 | 2010-10-27 | 大日本印刷株式会社 | Defect detection method for transparent gas barrier film |
| CN102707012A (en) * | 2012-05-11 | 2012-10-03 | 北京大学 | Narrow band thin-layer chromatographic sheet and preparation method thereof |
| CN102707012B (en) * | 2012-05-11 | 2014-12-24 | 北京大学 | Narrow band thin-layer chromatographic sheet and preparation method thereof |
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