Papers, ready-for-use plates, and flexible sheets for chromatography

Chromatographic Revie~,s Elsevier Publishing Company, Amsterdam Printed in The Netherlands

PAPERS, READY-FOR-USE FOR CHROMATOGRAPHY

P L A T E S , A N D F L E X I B L E SHEETS

K. MACEK AND H. BE~V~i~ovfl~ 3rd Medical Clinic, Charles University, Prague, and Medical Department, Charles University, Prague 6 (Czechoslovahia) (Received January 26th, 1971)

CONTENTS i. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2. Chromatographic papers . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3. Ready-to-use plates for TLC . . . . . . . . . . . . . . . . . . . . . . . . . . 4. Flexible sheets for TLC . . . . . . . . . . . . . . . . . . . . . . . . . . . . Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

I I 3 3 4 4

I. INTRODUCTION M a n y different m a t e r i a l s h a v e been i n t r o d u c e d into c h r o m a t o g r a p h y as a result of t h e increasing p o p u l a r i t y of p a p e r (PC) a n d t h i n - l a y e r c h r o m a t o g r a p h y (TLC) w i t h i n t h e p a s t few years s. I n m o n o g r a p h s d e v o t e d to these techniques, it is possible to find a s u r v e y of o n l y t h e m o s t c o m m o n p a p e r s a n d ready-for-use plates or foils. Unf o r t u n a t e l y , it is impossible to o b t a i n r a p i d a n d e x h a u s t i v e i n f o r m a t i o n r e g a r d i n g all kinds of m a t e r i a l s of this t y p e which are c o m m e r c i a l l y available. To m a k e the situation even m o r e confusing, in m a n y p a p e r s it is possible to find only t h e c o m m e r c i a l n a m e s of m a t e r i a l s used w i t h o u t a n y f u r t h e r details necessary for the r e p r o d u c t i o n of results r e p o r t e d in a p a r t i c u l a r paper. This was the reason w h y we t r i e d to s u m m a r ize d a t a on m a t e r i a l s which are in use in flat-bed c h r o m a t o g r a p h y . W e were u n a b l e to a v o i d gaps in the tables because some m a n u f a c t u r e r s d i d not answer our questions at all or their answers were incomplete. T a b l e r shows the m a n u f a c t u r e r s w h o m we approached. 2. CHROMATOGRAPHIC PAPERS B y t h e t e r m c h r o m a t o g r a p h i c paper, cellulose p a p e r is generally understood, a l t h o u g h p a p e r s of modified cellulose or glass fibre are also included. The m o s t w i d e l y used cellulose p a p e r is m a n u f a c t u r e d almost exclusively from the s h o r t e r c o t t o n fibres (linters)l, z. Chemically, the p a p e r consists of 9 8 - 9 9 % of a-cellulose, o . 3 - 1 . o % of r-cellulose, a n d 0.4-0.8% of pentosans. The p a p e r also contains a small p r o p o r t i o n of c a r b o x y l groups, which are responsible for the n e g a t i v e charge of the cellulose a n d its ion-exchange properties. I n addition, c u r r e n t c h r o m a t o g r a p h i c p a p e r s c o n t a i n small a m o u n t s of i m p u r i t i e s such as b o u n d amino acids (the nitrogen c o n t e n t is Chromatogr. Rev., 15 (1971) 1-28

2

K. MACEK, H. BE~VA~OVA

about 15 mg/ioo g of paper), various lipophilic substances (their amounts are usually given as the weight of the ether extract from the paper and consist of about 25 mg per IOO g of paper), and finally inorganic compounds (total ash content 0.04-0.07%). These substances usually do not interfere with the chromatographic analysis and need not be considered in most separations. The properties of the papers (made from raw materials of equal quality) are determined b y their structures. In paper chromatography, the height of capillary ascent is extremely important, as it influences the flow rate and the quality of separations. The thickness of the paper together with the weight is roughly the measure of the capacity of the paper. From laboratory experience, it is possible to conclude that in most separations the best papers are those which have a weight of 9o-12o g/m ~, a thickness of o.I6-O.22 m m and a height of ascent of 14o-25o min/3o cm. Such papers are called standard papers (Table 2). These papers are sold in the form of rectangular or circular sheets, or in special shapes. The commercial availability of such special shapes saves time and helps to give more reproducible results, as slight changes in the width of the paper at the point of entrance of the mobile phase m a y cause significant changes in the RE values. Some of the shapes of these papers are shown in Fig. I.

PATTERN

!

IIIIIIIIIII

CRL

KCT

Fig. i. Special patterns of Whatman chromatographic paper. In addition to the standard papers, which have approximately the same weight and flow rate, there is also a large group of papers made for special purposes. Among these there are the less dense papers for more rapid flow rates (Table 3), the slowrunning papers (Table 4), the so-called chromatographic cardboards for preparative use (Table 5), the acid-washed papers with a low ash content (Table 6), the specially hardened papers (Table 7) and papers free of lipid-soluble substances (Table 8). Papers with an increased exchange capacity have been introduced for use in the separation of substances of polar character. Good results can be obtained on ionexchange celluloses, such as carboxymethylcellulose, DEAE-cellulose, ECTEOLAcellulose, cellulose phosphate, cellulose citrate and others (Table 9; for review see ref. 7). Another possibility is represented by papers which contain different ionexchange resins (Table IO).

Chromatogr. Rev., 15 (1971) 1-28

PAPERS, READY-FOR-USE PLATES AND FLEXIBLE SHEETS

3

Other types of modified papers are those which have been recommended for the separation of some hydrophobic substances. For this type of separation, papers are used where cellulose is modified by acetylation or where the paper is treated with silicone oil (Table II). Another possibility is offered b y papers which contain adsorbents such as alumina or silica gel (Table 12). After cellulose papers, glass fibre papers have been employed more in recent years (Table 13). Their main advantages are that reagents which are too corrosive for cellulose paper can be used for detection, that the analysis is rapid, and that adsorption effects can be avoided in some cases. Many of these papers contain a large amount of silica gel and are also known under the not very suitable name of "instant thin layers ''3.

3. READY-TO-USE PLATES FOR

TLC

In spite of the great popularity of TLC, there was one point in this technique which, when compared with PC, was in the past a retrograde step: the preparation of the stationary phase was a long, time-wasting operation requiring a great deal of effort b y the laboratory worker and made high demands on laboratory space and equipment. I t is easy to understand that the individual preparation of plates was the main cause of the lower reproducibility of results. These were the reasons which some time ago stimulated the commercial production of ready-for-use plates (Fertigplatten). These plates use mostly thin glass as the supporting material and retain all the advantages of laboratory-made plates. However, in addition, they guarantee a higher level of reproducibility. Some of them contain an organic binder and are therefore abrasion-resistant so that it is possible to impregnate them b y dipping, and they can be marked with a pencil, etc. 4. The thickness of the layer is mostly 25 ° #m, but some producers offer layers from IOO #in to 1.5 ram. The plates are supplied with or without a fluorescing indicator. They are delivered in the standard sizes of 20 × 20 cm, 20 × IO cm and 20 × 5 cm. Some glasses are scored and can be easily split into smaller pieces. The time of development of precoated plates is generally substantially longer compared with laboratory-made layers. However, the quality of separation is usually better and for this reason it is possible to shorten the run. There are m a n y kinds of ready-to-use plates with a layer of silica get (Table I4), alumina (Table I5), kieselguhr (Table I6), florisil (Table i6), polyamide (Table 17, and cellulose and modified cellulose (Table 18).

4. FL E XIBL E SHEETS FOR TLC

Another type of material for TLC is precoated polyester sheets on a base of poly(ethylene terephthatate)l°, u. Also aluminium foil can be used as a support s. These foils have excellent reflective properties, which is of great importance in quantitative densitometric analysis. Sorbent layers of these sheets are usually thinner, usually of about IOO/zm thickness. In the case of silica gel, polyvinyl alcohol or solne other organic polymers are used as binders and occasionally the binding effect is improved b y a special treatment of the support surface 5,6. The sheets are easily

Chromatogr. Rev., 15 (I97I) 1-28

4

K. MACEK, H. BE~V2{ROV2~

m a n i p u l a t e d (cut) a n d are m a n u f a c t u r e d in s t a n d a r d dimensions (20 × 20 cm, 20 X IO cm a n d 20 × 5 cm). Quite recently t h e y have been m a r k e t e d in the form of rolls which p e r m i t separations of great length to be carried out 5. The flexible sheets are supplied with a layer of silica gel (Table I9), a l u m i n a (Table 2o), polyamide (Table 2I), cellulose a n d modified celluloses (Table 22) a n d p o l y c a r b o n a t e (Table 23). ACKNOWLEDGEMENT W e would like to express our deepest g r a t i t u d e to all m a n u f a c t u r e r s who, b y s u p p l y i n g us p r o m p t l y with d a t a relevant to their products, enabled this review to be published.

REFERENCES i A. GRUNE, Schweiz. Apotheker-Ztg., 93 (1955) 576, 587, 605. 2 A. GRONE, in If. MACEKAND I. 1Vi.HAIS (Editors), Stationary Phase in Paper and Thin-Layer Chromatography, Elsevier, Amsterdam, 1965, p. 15. 3 F. C. HAER, An Introduction to Chromatography on Impregnated Glass Fiber, Ann Arbor Sci. Publ., Ann Arbor, 1969. 4 H. HALPAAP,J. Chromatogr., 33 (1968) 144. 5 H. HALPAAPAND H. BAUSCH,J. Chromatogr., 48 (197o) 144. 6 H. HALPAAP, K. KLATYKAND H. ROSSLER, J. Chromatogr., 48 (197o) 163. 7 C. S. KNIGHT,Adv. Chromatogr., 4 (1967) 61. 8 K. MACEK (Editor), Pharmaceutical Applications of Thin-Layer and Paper Chromatography, Elsevier, Amsterdam, 1971. 9 K. MACEKAND J. HACAPERKOVA,Chem. Listy, 51 (1957) 895. lO E. P. PRZYBYLOWICZ,W. T. STAUDENMAYER,E. S. PERRY', A. D. BAITSHOLTSAND Z. ~. TISCHER, J. Chromatogr., 20 (1965) 5o6. I i V. R~BEK, J. Chromatogr., 33 (1968) 186. Chromatogr. Rev., 15 (1971) 1-28

TABLE 1 Company

Location

Analtech, Inc.

Blue Hen Industrial Park, S. Chapel Street Extension, Newark, Del. x97Ii, U.S.A. Phillipsburg, N.J. 08865, U.S.A.

j. T. Baker Chemical Co.

W. & R. Balston

J. C. Binzer Camag A.-G.

Cheng Ching Trading Co., Ltd. Carlo Erba S.p.A.

Gelman Hawskley Ltd.

Kavalier, n.p. Kodak Ltd.

Macherey-Nagel & Co.

Mann Research Laboratories

E. Merck A.-G.

Riedel-de Hahn A.-G.

Rohm and Haas Co. C. Schleicher & Schiill VEB Spezialpapierfabrik Niederschlag Stora Kopparberg Grycksbo Toyo Royishi

M. Woelm

H. Reeve Angel & Co., Ltd., 14, New Bridge Street, London, E.C. 4, Great Britain 3559 Hatzfeld/Eder, G.F.R. Homburgerstrasse 24, CH-4132 Muttenz, Switzerland Hankow Street, Taipei, Taiwan, Formosa Via C. Imbonati 24, 20159 , Milan, Italy i2 Peter Road, Lancing, Sussex, Great Britain Z~vod Votice, Czechoslovakia Eastman Kodak Co., Rochester, N.Y. 14650, U.S.A. 516 Diiren-R61sdorf, Werkstrasse 6-8, G.F.R. Division of Becton, Dickinson and Co., Mountain View Avenue, Orangeburg, N.Y. 10962, U.S.A. 61 Darmstadt, Frankfurter Strasse 25 o, G.F.R. 3o16, Seelze, Wunstorfer Strasse 4 o, G.F.R. Philadelphia 5, Pennsylvania, U.S.A. 3354 Dassel/Kr. Einbeck, G.F.R. Niederschlag/Erzgebirge, G.D.R. Grycksbo Pappersbruk, Sweden Nankano/Shima, Kita-Ku, Osaka, Japan 344 Eschwege, Postfach 840, G.F.R.

Representative in Europe or U.S.A.

j . T. Baker Chemicals N.V., Rijstenborgherweg 20, P.O. Box i, Deventer, The Netherlands

Camag Inc., 2855 South 163rd Street, New Berlin, Wisc. 53151 U.S.A.

Gelman Instrument Co., Ann Arbor, Mich., U.S.A.

Chemical Division, Kirkhy, Liverpool, Great Britain Brinkmann Instruments Inc., Cantiague Road, Westbury, N.Y, 11590, U.S.A.

EM Laboratories, 500 Executive Bvd., Elmsford, N.J. lO523, U.S.A. M.G. Scientific Gases, 240 Madison Ave., New York, N.Y., U.S.A.

Schleicher & Schflll, Inc., Keene, N.H. 03431, U.S.A.

Waters Associates Inc., 61 Fountain Street, Framingham, Mass. 01701, U.S.A.

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