Paper filters

The oxidation of black lead(II) sulphide to the white sulphate is a very sensitive test if the black sulphide is used as a stain on filter paper. 

The blackening of filter paper, moistened with a soluble lead(II) salt (e.g. the ethanoate or nitrate), by the formation of lead(II) sulphide. 

This reaction is a useful test for a sulphite or for moist sulphur dioxide, which turns dichromate paper (filter paper soaked in potassium dichromate) from yellow to green. 

Two layers of filter-paper are desirable for aqueous solutions for organic solvents, however, one layer is usually sufficient. 

When only a small quantity of solid material has to be filtered from a liquid, the small conical funnel C, usually known as a Hirsch funnel, is used in order to collect and drain the material on a very small filter-paper (see p. 68). 

The filtration of any solution through the ordinary conical funnel may be hastened considerably by the use of a fluted filter-paper, instead of one folded into quarters in the usual way. The folding of a fluted paper may be learnt far more readily by a demonstration in the laboratory than by any written description. 

Sometimes the crude substance may contain an insoluble impurity, and on cooling the solution it may be difficult to judge how much of the solid matter is merely undissolved impurity and how much is solute which has subsequently crystallised from solution. To avoid this difficulty, the hot solution should be filtered, and should thus always be absolutely clear before cooling is attempted. Therefore filter the hot solution into a clean tube through a very small fluted filter-paper contained in a correspondingly small glass funnel, which should have had its stem cut off as that shown in Fig. 6, p. 12 (and for the same reason). Unless the upper part of the filter is cut awav to reduce its size to a minimum, a large proportion of the solution will remain held mechanically in the pores of the paper itself and only a few drops of clear filtrate will be obtained. 

The crude organic material is placed in a porous thimble G (made of tough filter-paper), and the latter placed as shown within the inner tube C. The apparatus is then fitted below to a bolt-head flask H containing the requisite solvent, and above to a reflux water-condenser J. 

Whatman No. i filter-paper, and handled as little and as cleanly as possible. 

Both these acids are colourless, but the spots of each acid on a filter-paper strip show up in ultraviolet light as intense blue fluorescent zones. They can also be detected, but considerably less sensitively, by spraying with ethanolic ferric chloride solution, which gives with N-methylanthranilic acid a purple-brown coloration. 

Method. Prepare a paper strip from Whatman No i filter paper, as in the previous experiment, and draw a light pencil line about 3 cm. from the bottom cf. Fig. 25(B)). Mark three points A, B and C symmetrically on this line, if possible 2 cm. apart. Using the fine pipette, or a capillary tube, apply sufficient of solution (A) to the point A to give a damp spot about 0-5 cm. in diameter. Using a thoroughly washed pipette or a fresh capillary tube on each occasion, apply solution (B) and (C) to the points B and C respectively. Dry the strip in the air. 

When the solvent around the spot has evaporated, the plate is placed ertically in a glass developing tank (a cylinder for small slides) which contains a small quantity of the solvent and is lined with filter-paper dipping into the solvent the level of the latter is adjusted, preferably with a pipette, so that the lower edge of the absorbent layer is under the soh ent but the spot is above this level, and the top of the cylinder is then firmly closed. The solvent rises through the adsorbent layer, and the components of the mixture ascend at different rates depending on their affinities for the adsorbent. 

General Considerations. With liquids and solutions the most serious losses are due to (a) transference from spherical flasks and difficulties of drainage, (b) retention by filter-papers, (c) absorption by large corks. As containers for small quantities of liquids it is therefore often convenient to use pear-shaped flasks A and conical test-tubes or centrifuge-tubes B (Fig. 29). (In this and subsequent figures, approximate dimensions are given to indicate a convenient size.)... 

For the filtration of very small quantities of crystals, the simple apparatus shown in Fig. 46 is often used. It consists of a fine glass rod (sometimes termed a filtration nail ) which is flattened at one end, the flattened surface being preferably roughened. It fits as shown into a small funnel which replaces F (Fig. 45). A circular piece of filter-paper is cut e-g.y with a clean sharp cork-borer) so as to fit completely and snugly over the flat end. After draining, the nail is raised and the filter-paper and crystals are removed with forceps and dried. 

Now filter the ether through a fluted filter-paper directly into a 100 ml. distilling-flask, and then equip the latter with a 100° thermometer and a double-surface condenser to the end of the latter attach a receiver with a rubber delivery-tube precisely as before. Place the flask cautiously in a water-bath, the contents of which have previously been heated to about 60° at some distance from the apparatus arrange the depth of the flask in the water-bath so that the ether distils slowly over. Collect the fraction boiling between 34-39°. Yield, 25 g. (35 ml.). Not more than a verv small residue of etlianol should remain in the flask. 

Place 0 5 ml. of acetone, 20 ml. of 10% aqueous potassium iodide solution and 8 ml. of 10% aqueous sodium hydroxide solution in a 50 ml. conical flask, and then add 20 ml. of a freshly prepared molar solution of sodium hypochlorite. Well mix the contents of the flask, when the yellow iodoform will begin to separate almost immediately allow the mixture to stand at room temperature for 10 minutes, and then filter at the pump, wash with cold w ater, and drain thoroughly. Yield of Crude material, 1 4 g. Recrystallise the crude iodoform from methylated spirit. For this purpose, place the crude material in a 50 ml. round-bottomed flask fitted with a reflux water-condenser, add a small quantity of methylated spirit, and heat to boiling on a water-bath then add more methylated spirit cautiously down the condenser until all the iodoform has dissolved. Filter the hot solution through a fluted filter-paper directly into a small beaker or conical flask, and then cool in ice-water. The iodoform rapidly crystallises. Filter at the pump, drain thoroughly and dry. 

The oxime is freely soluble in water and in most organic liquids. Recrystallise the crude dry product from a minimum of 60-80 petrol or (less suitably) cyclohexane for this purpose first determine approximately, by means of a small-scale test-tube experiment, the minimum proportion of the hot solvent required to dissolve the oxime from about 0-5 g. of the crude material. Then place the bulk of the crude product in a small (100 ml.) round-bottomed or conical flask fitted with a reflux water-condenser, add the required amount of the solvent and boil the mixture on a water-bath. Then turn out the gas, and quickly filter the hot mixture through a fluted filter-paper into a conical flask the sodium chloride remains on the filter, whilst the filtrate on cooling in ice-water deposits the acetoxime as colourless crystals. These, when filtered anddried (either by pressing between drying-paper or by placing in an atmospheric desiccator) have m.p. 60 . Acetoxime sublimes rather readily when exposed to the air, and rapidly when warmed or when placed in a vacuum. Hence the necessity for an atmospheric desiccator for drying purposes. 

After about 20 minutes, when the liquid should be dry, filter it through a small fluted filter-paper into a 100 ml. distilling-flask attached to a water-condenser. Add some fragments of unglazed porcelain to the ethyl acetate, fit a 100° thermometer to the flask, and place the latter on a cold water-bath, which is then brought to the boil. Some ether is always formed as a by-product with the ethyl acetate, and by these means is carefully distilled off as a... 

When the ij hours boiling is complete, preheat a Buchner funnel and flask by pouring some boiling water through the funnel with the filter-paper already in position, and then quickly filter the boiling solution. Transfer the filtrate to a beaker to cool, and then wash the insoluble residue of diphenylurea on the filter twice with hot water, and drain thoroughly. Cool the filtrate in ice-water the monophenylurea separates as colourless needles. Filter at the pump and drain well. Recrystallise the crude product from boiling water, as in the previous preparation. Yield of monophenylurea, 2 5-3 g. m.p. 147°. 

In view of the small volume of nitromethane to be manipulated, the crude nitromethane may be extracted from the aqueous distillate with ether (30-40 ml.). Dry the ethereal extract over sodium sulphate, filter through a fluted filter-paper, and then distil off the ether on a water-bath with the usual precautions (Fig. 64, p. 163 Fig, 23(E), p. 45) finally distil the residual nitromethane. 

The benzene used in this preparation should be reasonably free from toluene therefore use a sample of benzene supplied by dealers as crystalUsable benzene, i.e.y one which crystallises readily when cooled in ice-water. It should preferably be dried over calcium chloride and, immediately before use, filtered through a fluted filter-paper. The pyridine should also preferably be dried over solid potassium hydroxide and redistilled. 

Dissolve 22-8 g. of ethyl crotonate in 40 ml. of dry carbon tetrachloride and add 35 6 g. of. V-bromosuccinimide. Heat the mixture under reflux for three hours. Cool to o and filter off the succinimide which is insoluble in cold carbon tetrachloride. Now shake the filtrate with water in a separating funnel, separate and dry the carbon tetrachloride layer with sodium sulphate. Filter through a fluted filter-paper into a Claisen flask and distil... 

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