Perkin triangle

For general work, a very satisfactory apparatus for collecting fractions under reduced pressure is the Perkin triangle C, which is shown in Fig. 14, together with the requisite fittings for the complete... 

G. A. R. Kon Jour. Chem. Soc.., 1930, 182) described a modification of the Perkin triangle having only two taps instead of the three described above. It may be purchased from Quickfit Quartz, Ltd., Quickfit Woiks, Stone, Staffs. 

The dotted line in Fig. 11,17, 2 refers to the modification of the apparatus for use in fractional distillation under reduced pressure a Perkin triangle or equivalent receiver device ( vacuum distilling adapter ) is generally employed for collection of the various fractions. 

Attach the flask containing the mixture, with capillary in position, to the column make sure that the Perkin triangle (or vacuum distilling adapter ) and receiver are in place. See that the oil pump is functioning... 

The chief disadvantage of the simple vacuum distillation set up shown in Fig. 11,19, 1 is that, if more than one fraction is to be collected, the whole process must be stopped in order to change the receiver B. It is of value, however, for the distillation of solids of low melting point the distillate can easily be removed from the receiver by melting and pouring out. For routine work, involving the collection of several fractious under reduced pressure, the most convenient receiver is the so-called Perkin triangle the complete apparatus for vacuum distillation is depicted in F g. 11,20, 1. The Claisen fla.sk A is fitted to a. short water... 

A set-up for distillation under reduced pressure is shown in Fig. 11,60,3 it is generally more convenient to use a Kon receiver or a Perkin triangle (Fig. 11, 56, 31). The vessel at the side, connected to the assembly by rubber pressure tubing, may be immersed in a Dry Ice-acetone bath and serves as a trap for volatile materials. 

Liberate the free base by adding to the phenylhydrazine hydrochloride 125 ml. of 25 per cent, sodium hydroxide solution. Extract the phenyl-hydrazine with two 40 ml. portions of benzene, dry the extracts with 25 g. of sodium hydroxide pellets or with anhydrous potassium carbonate thorough drying is essential if foaming in the subsequent distillation is to be avoided. Most of the benzene may now be distilled under atmospheric pressure, and the residual phenylhydrazine under reduced pressure. For this purpose, fit a small dropping funnel to the main neck of a 100 ml. Claisen flask (which contains a few fragments of porous porcelain) and assemble the rest of the apparatus as in Fig. II, 20, 1, but do not connect the Perkin triangle to the pump. Run in about 40 ml. of the benzene, solution into the flask, heat the latter in an air bath (Fig. II, 5, 3) so that... 

Fractional distillation under diminished pressure.—A 5-25 ml. Claisen flask (with pear-shaped bulb) provided with a fractionating side arm (Fig. II, 24, 4r-5) and attached to a Liebig s condenser and a Perkin triangle (Fig. II, 20, 1 or II, 20, 2 volume of receiver ca. 10 ml.) wUl be found to have wide apphcation. 

Apparatus. The generator employed is shown in fig. 10. There are six important points. (1) The column. <4 is designed so that throttling is avoided it is at least 2 ft. long and surmounted by a reflux doublesurface water-condenser B. (2) A Perkin triangle (air-cooled), inserted between the down-condenser and the traps, enables any phosphorus oxychloride which distils to be removed. (3) It is convenient to have three traps, viz. C, ice and salt D, acetone and carbon dioxide E, liquid air. (4) The intermittent addition of the solid antimony trifluoride presents a problem. The mechanical solid feed... 

Oglialoro modification of, 708 Perkin triangle, 108, 218f Kon modification of, 109 Peroxides, detection of, in ether, 163 removal from diethyl ether, 163 removal from isopropyl alcohol, 886 Petroleum ether, purification of, 174 Phenacetin, 996, 997 1 10-Phenanthroline, 991, 992 p-Phenetidine, 997, 998 Phenetole, 665,670 Phenobarbitone, 1003,1004,1005 Phenol, 595, 613 Phenol aldehyde polymers, 1016 formation of, 1022 Phenolphthalein, 984, 985 action as indicator, 984 ... 

The sinter filter is removed and dppe (7.32 g, 18.4 mmol), toluene (70 mL), and a magnetic stirrer are added to the filtrate. A Perkin triangle with a 12-cm Vigreux column is attached (Fig. 1). The Perkin triangle is a piece of apparatus which is used to remove volatile fractions from a boiling mixture. It includes a fractionating column to separate the most volatile fraction,... 

Figure 1. Reaction flask with Perkin triangle (A) 12-cm vacuum-jacketed Vigreux column, (B) oil bath on hot plate, (C) condenser, (D) thermometer, (E) extraction tap, (F) collection flask, (G) to nitrogen supply and bubbler.

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