Pour point apparatus

Certain calibrated orifice instruments (Engler-type) provide viscosity measurements at temperature lower than pour point. This is possible because the apparatus agitates the material to the point where large crystals are prevented from forming whereas in other methods, the sample pour point is measured without agitation. 

Figure 4.3. Apparatus for the determination of cloud point and pour point...

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... 

Place a mixture of 25 5 g. of n-valerio acid (Sections 111,83 and 111,84), 30 g. (37 -5 ml.) of dry n-propyl alcohol, 50 ml. of sodium-dried benzene and 10 g. (5-5 ml.) of concentrated sulphuric acid in a 250 ml. round-bottomed flask equipped with a vertical condenser, and reflux for 36 hours. Pour into 250 ml. of water and separate the upper layer. Extract the aqueous layer with ether, and add the extract to the benzene solution. Wash the combined extracts with saturated sodium bicarbonate solution until effervescence ceases, then with water, and dry with anhydrous magnesium sulphate. Remove the low boiling point solvents by distillation (use the apparatus of Fig. II, 13,4 but with a Claisen flask replacing the distilling flask) the temperature will rise abruptly and the fi-propyl n-valerate will pass over at 163-164°. The yield is 28 g. 

Mix 400 mL of pure concentrated hydrochloric acid with 250-400 mL of distilled water so that the specific gravity of the resultant acid is 1.10 (test with a hydrometer). Insert a thermometer in the neck of a 1 L Pyrex distillation flask so that the bulb is just opposite the side tube, and attach a condenser to the side tube use an all-glass apparatus. Place 500 mL of the diluted acid in the flask, distil the liquid at a rate of about 3-4 mL min-1 and collect the distillate in a small Pyrex flask. From time to time pour the distillate into a 500 mL measuring cylinder. When 375 mL has been collected in the measuring cylinder, collect a further 50 mL in the small Pyrex flask watch the thermometer to see that the temperature remains constant. Remove the receiver and stopper it this contains the pure constant boiling point acid. Note the barometric pressure to the nearest millimetre at intervals during the distillation and take the mean value. Interpolate the concentration of the acid from Table 10.5. 

The IEF mixture is poured between the gel plates up to the top and the comb is inserted (no stacking gel is required). Once the gel has set, the comb is removed and the wells are rinsed with distilled water. Any potential leaking points of the gel apparatus need to be sealed with 2% agarose as communication between the upper and lower chambers, must be avoided. 

Preparation of Chlorine by Oxidizing Hydrochloric Acid with Potassium Permanganate. Liquefaction of the Chlorine. Assemble an apparatus as shown in Fig. 54. Spill 10-15 g of potassium permanganate into flask 1. Pour a 37 % hydrochloric acid solution into dropping funnel 2, a saturated sodium chloride solution into cylinder 5, and a little concentrated sulphuric acid into wash bottle 4. Put the end of the gas-discharge tube of the apparatus into test tube 5 cooled outside by solid carbon dioxide (dry ice) wetted with acetone. What is the boiling point of chlorine ... 

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