DE2106689C3 - Thin layer chromatography elements and process for their preparation - Google Patents

Description

graphic is particularly suitable / ur la-nniuif from «lark adsorbent compounds, and requires only kur / c Chroma logriiphic / cil.

In an older, pre-published proposal (French patent specification I 543 724) in a process for the pretreatment of carrier foils, in particular polyester foils, in which a thin layer of a mixture of a sorbent, e.g. B. Kieselguhr. Aluminum oxide! or cellulose, and a thermoplastic resin, z, B, polyethylene powder, applied in the form of a thin liquid 'suspension and then at 60 to aufsinten! maximum of 18O ⁰ C. The product obtained is carrier foils for the production of thin layer plates for thin layer chromatography, that is to say intermediate products which are suitable for the application of sorbent layers.

The actual sorbent layer is placed on these carrier foils applied in a manner known per se exactly as in the known thin layer plates. This Sorption mills are therefore either mechanical insufficiently resistant or contained to improve mechanical resistance and adhesiveness an organic binder The quality of the actual chromalographically active sorption medium layer thus corresponds only the known Sorpiionsmittelschichten.

It was the object of the invention. Elements for thin layer chromatography / u create whose sorbent i-chichi is firmly connected in itself and with the carrier and is therefore mechanically resistant against abrasion or other damage and at the same time free of organic binders.

These elements should also be used with aggressive reagents can be treated and can be used for the qualitative or quantitative detection of faibioses organic compounds without any loss of quality the resulting recording. Furthermore, these elements are intended to be used repeatedly and regenerated can be without their chromatographic properties and their handling impaired will. After all, these elements should be firmly bound, uniform, strongly adsorbing chromatoeraphic Layers with high porosity and good reproducibility for chromatograpfmche Have separations on a preparative scale. A method for the production of elements is also intended for thin layer chromatography ensure that the elements produced have excellent wear resistance and the thin adsorbent layer, its ability to adsorb items to be chromatographed Retains substances even after repeated use and regeneration.

In the case of an element of the type mentioned at the outset, the object is achieved in that the binder consists of glass powder which is auigcsintered together with the sorbent.

The invention also relates to a method for producing the elements for thin layer chromatography by applying a layer of a mixture to which a volatile solvent has been added of an inorganic sorbent and a binder on c-; n thermally and chemically resistant Carrier, evaporating the solvent and heating the layer to a temperature hot the binder sinters, which is characterized in that glass powder is used as the binder.

VorziigswciMj becomes ills UimlcniiiHil Cilasptilver from Nalronkalkglaii. Uorsilikmglns, IJIcisilikalglas, U rar glas or gins with high SiQ.-Qeh.all used. who generally prefers glass powder of the same composition and physical properties as the carrier itself when using glass material as the carrier. In

In this case, a glass powder is preferably used, which has approximately the same particle size as the sorbent, this is added after the comminution Part of the Glaslrügers in a ball mill the powder by slurrying and sieving The particle size is fractionated and the particle size suitable for the particular purpose is selected. - In some lines, lilac silicate glass is preferred, because its melting point is much lower than that of glasses commonly used for wearers. A such glass is often advantageous because it is used for manufacturing "the element only requires moderate warming while heating, and thereby any possible impairment the chromatographic activity of the adsorption agent is reduced to a minimum and deformation of the carrier is avoided. As the inorganic sorbent, there can be various Substances are used, e.g. B. kieselguhr, aluminum oxide. Silica gel. Magnesium silicate or powdered porous glass. The particle size of the inorganic sorbent is usually so chosen that it is best suited for the purpose for which it is intended. Most of the commercially available sorbents for thin layer chromatography can advantageously be used without modification will.

Diatomaceous earth is particularly suitable because its chromatographic activity even after warming up or slightly above the melting point of soda lime glass (about 670 C) is not affected.

This results from the following experiments:

1. Different types of silica gel were presented before and examined after heating at 670 ° C. for 7 minutes. There was no difference in the specific Surface and the particle size distribution can be determined.

2. Thin-layer chromatography plates were after a conventional process using silica gel and heated to 670'C. Chromatograms with these plates were developed and were in no way worse than Chromatograms on freshly prepared pebble plates.

3. Electron micrographs of the sintered Plates confirmed that the porous structure of the sorbent was unchanged.

The glass powder and the sorbent are generally used in a weight ratio of 1: 1 up to 30: 1, preferably from 2: 1 to 10: 1, mixed. If the weight ratio of the sorbent to the glass powder is greater than 1: 1, the binding force is sufficient the particles in the layer are no longer out. On the other hand, a weight ratio is less than 1: 30 is not suitable as it leads to incomplete development. Parts by weight of the sorbent from 10 to 50 ",, of the weight of the total

mixture result voriclluilie hrgebmww. although the addition of such an envelope is ever.!

also other areas for certain additional areas · not necessary. Any volatile solvent, φ

Positions of sorbent and fluid, including water, can be used with kneading. }

can be suitable use! will. Bm the use of W »sscr]

-Hgcmein decreases with increasing weight decreases- δ see infrared radiation / from fast H.

• m; From glass powder to sorbent the R / * value dampen the remaining water. In nc wish «<«, | /

tjes property of the solvent developed with a given solvent is dm ! ability, Φν - _: \ η

Chromatogriimms too. whereby the R, -Weri is left undislwi 211 through the erve «/, hurried layer until j g

Rucdrigung the polarity of the Laufmi'ticU can be influenced it is sintered. S.

is. Therefore, there are strongly polar substances, which m The applied ■ "<'dried layer is shown in J f

up to now difficult to separate chromatographically, an electrical OK .1 a few minutes at the tem- _ · f

Easily separate on a plate of the invention, at the perü '. <r at which the üias begins to melt, or

the activity of the sorbent by changing at a slightly lower temperature

the weight ratio is set. This represents sintsrl. t ^; For simple soda-lime glass plaUs this lies

a surprising advantage of the invention. 15 suitable temperature at about 650 to 700 "C. H the

The carrier can be made of refractory and chemically temperature too high, the -aim layer melts and permanent materials such as glass, metal or ceramic are destroyed, while if the temperature is too low and has the shape of a plate, usually no sintered layer is formed , him Erhilzungszcit a rectangular plate. Same or of the kind of about 10 minutes is sufficient to solidify each glass powder. '... these glasses are to be formed in the same way - 20 bound Sinlersdn,
moderately usable. 11 .1η- corrosion-resistant steel After the rear. -Earth the plates lengthways or aluminum are suitable examples for chemically cooled. Regardless of the fact that an elwa resistant metals, but also other metals, z. B. tenfold difference between thermal out-iron, copper and brass, can be used, expansion coefficients of the glass and the sorption when there are some restrictions / u maciien, which exists by means of, for example, the Ausdc! < 'npskocffiauf the chemical reactivity with the too cient of Naironkalkglas elwa 9.? ...! O *, vo'i silica gel chromatographicrende material ■ - ¹ Jr with the used but about 5.4-10'), form the particles of the sinter inverted Eluents are returned. Steatite is a solid and mutually fused bin in the preferred ketan-i-cnes maierial. fertilize.

According to the method of molding, the layer of powdered glass that makes up the plate

Gernisch shaped from glass powder and derr- sorbent;. , 11 · «r covered, results in a pure white,

after adding a small amount of a volatile sponge-like structure with many small intervening

Solvent, e.g. B. Benzene, alcohol, acetone, water clear or voids, and it is believed

or a mixture thereof, kneaded. The so that the adsorbing particles within the intermediate

The pulp formed is held with the help of a customary application or cavities, without being leak-proof

Device applied to the carrier and about to be packed together. This ai view is through

this distributed. The thickness of the layer applied supported the fact that the chron ^ graphic

Layer sufficient for plate or thin-layer chromatography activity of the sorbent

chromatography can 150 μ to 2 mm be even after the sintering or firing is maintained.

In one of the exemplary embodiments, the slurry 40 if the adsorbing <* n particles in the sintered layer

with one for the application of a damp layer of completely molten glass fc *. licks

The expected activity of the sorbent would go to a suitable application device 500 μ thick

Carrier applied and presumably lost over its surface,

Splits. The thickness of the sintered layer on the _{Dje Qü je) e} , _{ä fe dje invention} .

Trager is formed, can be 200 to 300 μ. 45

With such layer thicknesses, the deviation remains Example 1

of the R / value of the chromatogram within the ,, ",. ,. .

Error area of the development process. ^A - Preparation of the chromatographic plates

Other auxiliaries can optionally be added to the glass from commercially available soda-lime glass supports if they do not leave any residue in the plates for thin-layer chromatography after firing. Such an additive can be comminuted to a gel in a ball mill. After mixing the sludge, the appropriate strength, consistency and sieving of the comminuted product is obtained or has viscosity. Canadabalsarn, which is a very fine glass powder with particle size-related properties, can z. B. to the division of 14% 1 to 2 μ, 23% 2 to 3 μ and 18% j mixed preferably be added, since it meets the different 55 3 to 4 μ and with a specific surface area of I different conditions and as this is 3.4 m ² / g · I solution section! benzene used is sufficiently volatile. The glass powder is coated with silica gel for the chroma- |

An aqueous starch solution can also be used as an additive in the formulas given in Table I.

can be used, but such organic weight ratios are mixed. 20 g of the firm G? -

Substances sometimes to stains or blackening 60 mix v / ground with 200 g Canada balsam and 60 ml

. of the sintered plate due to carbonization. Added to benzene and kneaded into a doughy paste,

Similarly, in some cases polyvinyl The slurry is applied with a conventional application device

alcohol or polyacrylamide can be added. When applied to and spread over glass plates.

.the sample to be chromatographed is not insoluble. The glass plates are made of the same material

Sulphate or calcium salt forms, gypsum can without 65 like the glass powder. The dried plates are

substantial difficulties zl -i / will be. Then in 10 minutes at 680 ° C in an electric

In this case, a relatively thick layer of oven can be heated with success. This creates white sintered layers

up to 2 mm can be formed. made of glass powder with the sorbent silica gel.

B. Results of development and separation attempts

In order to test the release effect of the plates produced in this way, a series of development tests is carried out with 3 estrogens as comparison substances to be chromatographed accomplished.

Conditions for ascending development: temperature: 20'C (room temperature); Solvent: Benzene-ethyl acetate (2: 1); Running distance: 10cm; Time: 18 to 21 minutes; Contact point: 2 crr. from the bottom.

Table 1

Sorbents and be Oestrone R / value Estriol Weight ratio
to the glass powder 0.67 Östra
diol 0.09 Silica gel H 1: 1 0.74 0.55 0.09 1: 2 0.76 0.59 0.09 1: 3 0.78 0.60 0.10 1: 4 0.66 0.63 0.06 layer PH 1: 4 0.71 0.48 0.09 1: 5 0.79 0.55 0.12 1: 6 0.83 0.64 0.14 1: 7 0.86 0.72 0.15 1: 8 0.88 0.72 0.16 1.9 0.88 0.76 0.17 1:10 0.94 0.76 0.36 1:20 0.79 0.88 0.08 1: 20 *) 0.46 0.66 0.10 Silica gel H alone **) 0.30

*) In general, with an increasing ratio of glass powder to sorbent, the R / value increases with a given solvent. The polarity of the eluent can be reduced by using benzene-ethyl acetate (4: 1. The R _r value can be influenced by changing the solvent polarity. **) These results on thin-film chromatographic plates which were produced only from Kicselgel H according to a conventional process, are comparatively given. Benzene-acetic acid ether (2: 1) was used as the mobile phase.

C. Reproducibility of development and separation properties of the plates

The chromatographic plates are produced according to the method described under A, glass powder / u sorbent 4: 1; Sorbents a) Kicselgel H or b) layer PH], developed and on made visible in the usual way. Then they are soaked in bichromate sulfuric acid, with Washed out distilled water and repeated after reactivation by heating to 100 "C for one hour Regenericrungsversuche subjected.

The results of repeated development tests are listed in Tables II and IN. Of course, it must be washed out and reactivated after each attempt. A loss of activity of the thin-layer chromatographic plates could not be determined after at least five attempts will.

Comparable substances: 3 estrogens; Conditions for ascending development: temperature: 20C (room temperature); Running track; 10 centimeters; Aufsetzstellec: 2cm from the lower edge; Solvent; Benzene-ethyl acetate (2 : 1).

Table U
a) Sorbent: Kicselgel M

Attempt no.
5 'Oestrone R / -Wcri
ösna-
-.fiol Estriol Time,
Minutes 1 Ό, 75 0.60 0.0 « ; ■ - - ■
20th 2 0.74 ' 0.5S 0.09, 0.76 0.59 ■ Ό. 1.0 -.UO. r ^Io 4 0.75 0.5S ο.ιο -: 20 Γ 5 0.70 0.54 0:09 .20 Average 0.74 ' 0.58 0.09 ... . .- .. 20, σ>) 0.02 0.02 0.01 ■ -

* ■) ff Standiirdabwcichiing.

Table 111 b) Sorbents: layer Pll

Attempt no. Oestrone R _r -Wcrt
Östra
diol Estriol Time,
M'niilen 1 0.71 0.57 0.09 20th 2 0.70 0.58 Ο, ΪΟ 21 3 0.72 0.60 0.08 21 4th 0.73 0.60 0.07 21 5 0.66 0.48 0.07 10 Average 0.70 0.57 O.OS 20.6 σ 0.03 0.05 0.04

As can be seen from Tables M and III, the sintered plates are suitable for repeated use and show good reproducibility after tien individual regenerations.

Example 2

ChrorrvUogniphic plates are more similar Way as described under A, Example 1, hcrges: ellt, where al; Porous glass powder with sorbent

high SiO ₂ content, in a mixing ratio of 4: 1.

Tine series of similar developments, as in the Example 7 (C) is described, using three estrogen as a balancing substance and

Bcr.zol-Lsigsäureitthvlestcr (10: 1) as eluent accomplished. The results are shown in Table IV.

Table IV

Try Ni. oestrone R / -Wer (
Östra
diol Estriol Time.
Minutes 1 0.62 0.36 0.02 22nd 2 0.64 0.37 0.02 22nd 3 0.64 0.37 0.03 23 4th 0.60 0.37 0.02 ' '22 5 0.63 0.37 0.03 22nd Vlitlclwcii 0.62 0.37 0.02 .- 22.2 σ 0.03 0.01 0.01 -

Hei a lowering of the polarity of the Laufmittel.s to compensate for the relatively small specific, Oberlliichc of the porous glass powder, J55 m- / g (the vOiI Kiciülßcl amounts to 500 ^s / fi in general) and [ieuiiiflussuiigidcr R / AVcrle. becomes, no negative effect in Chromatouramin or in the Trennfüliigkcit (chromalographi.sdic activity) bcohachicl.

609625/144

Example 3

Chromatographic plates are prepared in a manner similar to that described under A, Example Ϊ. Alumina, sorbent and glass powder were used in a weight ratio of 1: 4. Then Zn ₂ SiO ₄ -Mn is added in an amount of 2% of the total amount as a fluorescent agent.

A series of repeated developments is carried out on the panels so produced and on after one plates manufactured with Merck Alumina HF using various conventional processes Alkaloids carried out as comparison substances to be chromatographed. The results and compiled in Table V:

Conditions for ascending development: temperature: 20 ^° C. (room temperature); Mobile phase: benzene / chloroform-diethylamine (9: 4: 1); Running distance: 10 cm; Time: 25 to 26 minutes; Contact point: 2 cm * from the lower edge; Evidence: UV irradiation (254 πιμ).

Table V

alkaloid

Codeine ...
Thebaine ...
Atropine ...
Yohimbine.
Reserpine ..
Ergotamine

Brucine

Strychnine ..
Nicotine ...

quinine

Cinchonine
Aconitine ..
Emetine ...
Caffeine

R / value (sorbent)

Alumina with glass powder

0.54 0, fa2 0.49 0.44 0.58 0.28 0 /> 7 0.72 0.80 0.55 0.57 0.73 0.76 0.48

Alumina alone

0.50 0.90 0.55 0.43 0.68 0.23 0.71 0.73 0.82 0.46 0.59 0.78 0.75 0.59

Example 4

In a manner similar to that described under A, Example 1, chromatographic plates are made. In this example, however, no auxiliary binders are used used as additives. 16 g of fine glass powder are mixed with 4 g of silica gel and after Addition of 34 ml of ethanol kneaded.

Table VI shows the results of development tests on plates produced in this way Compared to plates made with silica gel in the usual way.

Conditions for ascending development: temperature: 20 ^° C. (room temperature); Mobile phase: benzene-ethyl acetate (2: 1); Running distance: 10 cm; Time: »20 minutes; Aufsetzstelje: 2 cm from the lower edge; Comparative substances: ■■ estrogens.

Table VI

\. Flat style Oestrone R _r value
Östra
diol estriol sintered panels
\ , -Example 4,. ,,.,.
'After a usual
Γ Process manufactured
"Kiesejgei-Piatte 0.76
0.46 ' 0.63
0.27 0.10
0.10

Example 5

In a similar way as described under Λ, Example I, fine glass powder is produced, but in the> em example lead silicate glass is used instead of NutrijiikulkHas is used.

'Jas so lier.ueslclltc Gla.spiilver has the following particle sizes distribution: 14 °;, I to 2 jx. 29 ",, 2 to 3 µ and 21" "3 to 4 µ. The specific surface is cheating ? .i mVs? ·

The glass powder is then mixed in a 3: 1 ratio with Kicsclücl and kneaded iterially with 2.0 ml of ethanol / g of solid material to form a paste. The paste is applied in an amount of about 10 g / 100 cm ² to rectangular Na'.ronkiilkglaiplatlen (5 x 20 cm, 1.2 mm thickness) with a conventional application device. distributed. The dried plate is then fired for 3 minutes in an electric oven at 560 ° C., whereby a white layer of glass powder (170 μ thick) is formed, which encloses the sorbent silica.

In order to test the separation properties of the plates obtained and the reproducibility after repeated use and regeneration, a series of development tests are carried out according to the procedure described above. Regeneration can be carried out by soaking the used plates in a bichromate / sulfuric acid bath for five hours, after which they are washed with water and ^{reactivated at 110 °} C. for 30 minutes. The test results are shown in Table VII.

Comparative substances: estrogens.

Conditions for ascending development: temperature: 25 ° C. (relative humidity: 50 to 60 " _o ); running material: benzene-acetic acid ethyl acetate (2: 1): running distance: 10 cm; time: 15 minutes; landing stage: 2 cm

from the bottom,

Reproducibility of the hR / AVertc ^ Table VI hR / ~ W'.rl Estriol östra
diol 10 40 number of 55 η
V Regenerations 50 8th 0 51 O 45 1 59 S. 2 54 8th 3 53 9 4th 53 8th 5 51 30th 50 6th 60 'ό 7th 52 8.7 8th 53.8 0.8 9 3.5 9 ± 1 55 Mr} 54 ± 4 σ **) Repioduzicrbnrkcit oestrone 69 r s
OO 66 74 69 67 66 65 73 65 68.0 3.2 68-Jr 3

*) jiJV value: crmiiiclicr R> value x 100;

hR / - \ Vcri: arithrnciisclics means; ms i0 **) ff: Siandarcfabwcichiing der lOhli / AVcrtc, In the case of usual thin-section chromntograpliic is also

with closer control of the factors' the. the rcpro

can influence manageability, a Slieui'ing u »)

the experimentally determined hitJ-Wsrt by --- 5 z.-

6g casual.

Huthaken the chromatographic plates prepared according to this example as part of the Blcisilikalgluscs a fluorescent agent, so can

Ll

they are used to make an examination material visible with absorption in the UV range according to the so-called «Quencru method used as with the usual thin-layer chromatography (produced e.g. by applying silica gel or aluminum oxide with a fluorescent agent). In addition, these plates are suitable for regeneration, because the inorganic fluorescent agents enclosed in the lead silicate glass by the heat treatment or by spraying on hot concentrated sulfuric acid or bichromate sulfuric acid cannot be deactivated.

Example 6

In a manner similar to that described under A, Example 1, fine glass powder is produced. In this example, however, a type of uranium glass with 1.8% U ₃ O _{8 is used} instead of soda-lime glass. It has a particle size distribution of 18% 1 to 2 μ, 37% 2 to 3 μ and 15% 3 to 4 μ and a specific surface area of 3.8 m ² / g.

0.45 g of the fine powder are then mixed with 3 g of powdered soda lime glass from Example 1 and 1 g of silica gel and, after adding 8 ml of acetone, kneaded to form a thick paste. The paste is then applied to rectangular soda-lime glass plates (5-20 cm, 1.2 mm thick) with the aid of an applicator and spread. The dried plates are then sintered in an electric furnace at 670 ^{° C. for 3 minutes.} White sintered layers of glass powder with a thickness of about 200 μ arise, which contain the sorbent in a homogeneous distribution and when excited with UV light of 253.7 μm show a greenish-yellow fluorescence.

One of these plates is made using testosterone as a well-known prefabricated plate fluorescence quenching material compared.

The reproducibility of the development and separation properties of the plates in such a quenching process is shown in Table VII! compiled. To determine the R / values, the spots are made visible in UV light of 253.7 μm or blackened after spraying with concentrated sulfuric acid. For regeneration for further use v / ground the developed plates in a "bichromate-sulfuric acid bath soaked 1 hour, washed and reactivated at HO ⁰ C 30 minutes. Test substances: steroids.

Conditions for ascending development: temperature 25 ^° C. (relative humidity 50 to 60%); _{$ 0} mobile phase: chloroform-acetone (4: 1); Running distance: 10 cm; Attachment point. · 2 cm from the lower edge.
Table VIII

Example 7

A. Manufacture of Chromatographic Plates

1. Glass powder -;

In a manner similar to that in Example 1 (A) be ^ wrote, two types of glass powder will follow-! made so: '"

a) Soda-lime glass with a particle size increase ·, '■■. division of 13% 1 to 2 μ, 25% 2 to 3 μ and "'18% 3 to 4 μ and a specific surface area of 3.5 m ² / g.

b) lead silicate glass: consisting of 59.6% Pb ₃ O ₄ , 13.5% SiO ₄ , 23.1% B ₄ O ₃ , 1.5% Al ₂ O ₃ and 2.0% Na ₂ O; Particle size distribution: 14% 1 to 2 μ,

₂ g

28% 2 to 3 μ and 22% 3 surface area: 3.1 m ² / g.

g% μ,

up to 4 μ; specific

35

40

number of hR / *) - value of the steroid , Testo
sterone Proge
sterone Regenerations Cortisone 59 68 0 37 60 73 1 40 57 71 2 35 54 73 3 37 60 74 4th 40 58 72 fiR / 38 3 2 σ *) 2 58 ± 3 72 ± 2 reproducibility 38 ± 2

55

6o

2. Used sorbent

c) alumina.

d) silica gel.

3. Carrier: rectangular plates, 50 x 200 mm titanium (TP 35), 1 mm thick;
corrosion-resistant steel according to 27), 0.5 mm thick;

Aluminum (ALP 1 - 0), 1 or 2 mm thick; Iron (SS 41), 1 mm thick;
Brass (BSP ₃ - 1/4 H), 0.5 mm thick; Steatite, 2 mm thick.

One of the glass powders a) or b) and one of the sorbents c) or d) are mixed with one another in a weight ratio of 16 to 20: 4 g. After adding 40 ml of acetone (about 2 ml per gram of solid mixture), the mixture is kneaded to form a dough-like paste. Each slurry is then applied to four supports of each material (3) (total surface 400 cm ² ) and distributed with the aid of a conventional application device. The dried panels are sintered in an electric furnace. Sintered layers of glass powder are obtained which contain the sorbent in a homogeneous phase.

The sintering can take in soda 10 to 20 minutes at 650 to 700 ⁰ C. When aluminum = slabs coated with the slurry, the sintering time must be shortened to 8 minutes at 650 C ^3. The sintering time can be shortened as a binder to 2 minutes at 450 ⁰ C with the use of lead silicate glass.

B. Results of developmental and separability studies

In order to determine the separability of the panels produced according to the above procedure, a series of development studies under “Use. a mixture of azo dyes or estrogens i carried out as comparison substances .: Both Sjuh-; Punch classes result in good chromatographic separations. The results are given in Tables IX, X and XI.

“· *) The characters hR / -, JiR, and σ have the meaning given in table VJI.

Investigation 1

. 6s conditions for ascending development: tem- 'perature: 25 ° C (relative humidity 50%); sorbent: silica gel; Laufmjttel :, benzene; running distance: cm 10.

13th

Table JX

14th

carrier

Glass ratio R _r value of the azo color
Indophenol j Sudan red GI Bullcr yellow

Time, minutes

titanium

corrosion-resistant steel ..

Aluminum (2 mm)

Aluminum (1 mm) .....

E se ι

Vesiing

S'eitit

finished panel

N-K. *) (1: 4)

N-K. (1: 4)

N-K

B *)

Ν — Κ

N-K N-K

(1: 5) (1: 4) (1: 4) (1: 4) (1: 4) 0.12
0 _v 10
0.11
0.10
0.08
0.08
0.06
0.05

0.22
0.22
0.29
0.21
0.20
0.20
0.17
0.13

0.55 0.55 0.58 0.57 0.46 0.50 0.40 0.38

20 20 18 18 17 17 29 25

*) N-K: soda lime glass, B: blown silicate glass.

examination

Conditions for ascending development: Eluent: benzene-ethyl acetate (2: 1); Proof: by carbonization with concentrated sulfuric acid; Silica gel: soda lime glass = 1: 4; (the other Examination conditions are the same as in Examination 1).

Examination 3 * ⁵

Conditions for ascending development: Running means: Carbon tetrachloride; Carrier: titanium; Aluminum oxide: Soda lime glass = 1: 4. (The other search conditions are the same as in Investigation 1.). ',

carrier

_{T {tan}

more corrosion resistant
steel

R / value of estrogen '<W, I oestrone

estriol,

0.15

0.13

.Time, minutes

0.65

0.62

0 "5

0.76

Table Xl

indophenol Sudan Red O R / -Wcrt of the azo dyes
ι
Äzoöcfrze! j Sudangeib
I. Buttergslb p-amino
a7obcnzoi Time,
Miffiilcil 0.10 0, V 0.18 j 0.48 0.50 0.80 32

Claims (10)

Patent claims: 1. Elements ϊιιγ Plinnschichlchromdiogriipliic, consisting of a thermally and chemically resistant trailer on which a mixture of one! inorganic sorbents] and a binding agent in thin shoes. is, by it characterized in that the binder consists of glass powder which is sintered up together with> o the sorbent. 2. Elements for Dünnschichtchromntog.raphie according to claim I, characterized in that the glass powder made from soda-lime glass, borosilicate glass, Lead silicate glass, glass with a high SiCV content. Uranium glass or a mixture of these glasses considered. 3. Elements for Dtjnnnschichtcnromatographie according to claim I, characterized in that the carrier from. Glass, metal or ceramic. 4. Elements for thin-layer chromatography "'according to claim I, characterized in that the sorbent consists of silica gel, aluminum oxide, Diatomite, magnesium silicate or porous glass powder with a high silicate content. 5. A method for producing the elements for thin layer chromatography according to claim 1 by applying a layer of a mixture to which a volatile solvent has been added from an inorganic sorbent and a binder to a thermal and chemically resistant carrier, evaporating the solvent and heating the layer to a Temperature at which the binder sinters, characterized in that the binder Glass powder used. 6. The method according to claim 5, characterized in that the sorbent used is silica gel, Aluminum oxide, diatomaceous earth. Magnesium silicate or porous glass powder with a high silicate content "uses, and this pulverized and sieved before mixing with the glass powder. 7. The method according to claim 5 and 6, characterized in that glass powder made of soda-lime glass, Borosilicate glass, lead silicate glass, uranium glass or glass with a high SiO content are used and makes the particle size of the glass powder similar or equal to the particle size of the sorbent by slurrying and sieving. 8. Process according to claims 5 to 7, characterized in that one is used as the solvent Benzene, a ketone, an alcohol, water or mixtures thereof are used. 9. The method according to claims 5 to 8, characterized in that the carrier glass, Metal or ceramic used, shaped into a rectangular shape before the mixture is applied would. 10. The method according to claims 5 to 9, characterized in that one is a mixture «Us sorbents, solvents and binders with an additional content of one Auxiliary binders, preferably Canada balsam, are used. 65 The foundation meets elements of thin-layer chromatography consisting of a thermally and chemically resistant Triigcr on which a mixture is applied from an inorganic sorbent and a binder in a thin layer and a Process for their manufacture. DOnnschichlehromatograpliic procedures are becoming more and more widespread in analytical chemistry. They are easy and quick to perform and are suitable for a large number of separations, through a large selection of sorbents, the convenient introduction of other components, e.g. fluorescent or complexing agents, and the change of conditions, e.g. B. the eluent, there are a number of parameters 7. \\ r , which can be used to achieve the desired separation. A major obstacle to the further spread of thin layer chromatography is that the previously known elements for thin layer chromatography were fragile and showed signs of wear and tear showed. Common chromatographic elements consist of a glass plate covering a thin layer a loosely adhering absorbent powder. They are commercially available but will, as the Prefabricated layers are fragile, and are very easily damaged in packaging or shipping. In addition, they are unsuitable for storage and recording purposes as they are resistant to wear and tear Are fragile. As a result, the plates are mostly just before use coated. In this case, disadvantages must be accepted, such as troublesome operations when mixing the sorbent and the binder, when dispersing the mixture in a liquid dispersion medium, when kneading the dispersed mixture into a slurry and when applying it to the Carrier in a homogeneous layer. Insufficient homogeneity of the pulp and insufficient uniformity the sorption layer, which depends on the different skill levels of the workers who manufacture the elements, have a considerable influence on the reproducibility of the experimental Results. In addition, known elements for thin layer chromatography, the organic substances, such as starch, polyvinyl alcohol, agar-agar or polyacrylamide as binding components contain the The disadvantage that they are subject to thermal visualization with aggressive reagents such as sulfuric acid, Cannot withstand nitric acid, iodine or bichromate sulfuric acid. These reagents are suitable to make numerous colorless organic compounds visible, but they can be used in one Such a composition of the chromatographic elements should not be used as they often take the background discolor the developed spots. On the other hand, chromatographic elements which plaster of paris can be used as Containing binders, not used for the detection of active compounds that form sulfates or calcium salts will. From the Chemiker-Zeitung, chemical apparatus / process engineering, Vol. 93 (1969), No. 9, pp. 329 to 332, silica gel glass fiber fleece layers are known which contain the sorbent silica gel incorporated into a glass fiber fleece without the addition of binders. This layer material for thin layer chromatography