Pyrex

The reports were that water condensed from the vapor phase into 10-100-/im quartz or pyrex capillaries had physical properties distinctly different from those of bulk liquid water. Confirmations came from a variety of laboratories around the world (see the August 1971 issue of Journal of Colloid Interface Science), and it was proposed that a new phase of water had been found many called this water polywater rather than the original Deijaguin term, anomalous water. There were confirming theoretical calculations (see Refs. 121, 122) Eventually, however, it was determined that the micro-amoimts of water that could be isolated from small capillaries was always contaminated by salts and other impurities leached from the walls. The nonexistence of anomalous or poly water as a new, pure phase of water was acknowledged in 1974 by Deijaguin and co-workers [123]. There is a mass of fascinating anecdotal history omitted here for lack of space but told very well by Frank [124]. 

Borax is used in the production of pyrex glass, ceramics, as a flux in soldering and welding, and in laundering to impart a glaze to linen. 

Apparatus. The apparatus is made of Pyrex glass, in one piece. It consists of a shaped bulb A (Fig. 89 of about 30 ml. capacity in which the reaction takes place, provided with an inclined inlet B at the side and a vertical ascension tube D. B serves not only as an inlet for the admission of the carrier gas but also as the route by which the reagents and test sample are introduced into the apparatus. B ends in a small ground-glass joint into which fits ajoint carrying a capillary-tube which projects well down into the bulb A (the end of the capillary should be just above the liquid level when the apparatus is charged for the determination). The upper extension of this capillary beyond the joint is provided with a tap C to control the rate of flow of the carrier gas. 

In the Pyrex glass West condenser greater efficiency of cooling is obtained by having a light-walled inner tube and a heavy-walled outer tube with a minimum space between them. 

Pyrex glass is preferable, but this requires an oxy-coal gas blowpipe for manipulation. Suitable melting point tubes may be purchased from dealers in scientific apparatus or chemicals. It is, however, excellent practice, and an essential part of his training, for the student to learn to prepare bis own capillary tubes. 

For solids which melt above 100° and are stable at this temperature, drying may be carried out in a steam oven. The crystals from the Buchner funnel should then be placed on a clock glass or in an open dish. The substance may sometimes be dried in the Buchner funnel itself by utilising the device illustrated in Fig. 77, <33, 1. An ordinary Pyrex funnel is inverted over the Buchner funnel and the neck of the funnel heated by means of a broad flame (alternatively, the funnel may be heated by a closely-fltting electric heating mantle) if gentle suction is applied to the Alter flask, hot (or warm) air will pass over the crystalline solid. 

Anhydrous sodium sulphide. The hydrated salt, NajS.QH O, is heated in a Pyrex distilling flask or retort in a stream of hydrogen or of nitrogen until water ceases to be evolved. The solid cake of anhydrous sodium sulphide is removed from the vessel with the aid of a copper wire hook or by other suitable means. No attempt should be made to fuse the sodium sulphide since at high temperatiues sodium sulphide is readily oxidised to sodium sulphate. 

AU ground glass joints should be constructed of a high resistance glass, such as Pyrex. The most common form is shown in Fig. II, 55, 1, and this is the type largely encountered in practice. Fig. II, 55, 2 is... 

The Stedman-type column is shown in Fig. 11, 56, 25. The characteristic features are (i) the use of a fine stainless steel wire cloth formed into conical discs, and (ii) an accurately fitting Pyrex glass jacket, produced by shrinking Pyrex glass on mandrels to the required inside dimensions. Modifications incorporating a silvered vacuum jacket and an electrically-heated jacket are marketed. This column is said to possess high efficiency but is expensive. It is generally employed in conjunction with a total-condensation variable take-off still head. 

Pack the catalyst into a Pyrex combustion tube about 90 cm. long and 15 mm. bore, and place plugs of glass wool at 25 cm. intervals inseit into a tube furnace and adjust to a temperature of 330° full details of the complete apparatus are given in Section 111,72 and Fig. Ill, 72, 1. 

Mix 100 g. of maleic acid (Section 111,143) and 100 ml. of tetra chloroethane in a 250 ml. Claisen or distilling flask provided with a thermometer, and attach a Pyrex Liebig condenser. Heat the flask in an air bath (Fig. 11, 5, 3) and collect the distillate in a measuring cylinder. When the temperature reaches 160°, 76 ml. of tetrachloroethane and 15-15-5 ml. of water are present in the receiver. Empty the water in the condenser and continue the distillation change the receiver when the temperature reaches 190°. Collect the maleic anhydride at 195-197°. Recrystallise the crude anhydride from chloroform. The yield of pure maleic anhydride, m.p. 54°, is 70 g. 

Reflux a mixture of 1 g. of the ester, 3 ml. of benzylamine and 0 1 g. of powdered ammonium chloride for 1 hour in a Pyrex test-tube fltted with a short condenser. Wash the cold reaction mixture with water to remove the excess of benzylamine. If the product does not crystallise, stir it with a httle water containing a drop or two of dilute hydrochloric acid. If crystallisation does not result, some unchanged ester may be present ... 

Prepare the acetaldehyde solution by plunging a red hot oxidised copper coil (made by winding a copper wire round a glass tube and heating the resulting coil in a Bunsen dame) into 6 ml. of 60 per cent, alcohol in a Pyrex test-tube. Withdraw the coil, cool the test-tube under the tap, repeat the oxidation several times, and use the cooled solution for the test. 

Place 0-5 g. of the amino acid and 1 0 g. of phthalic anhdride in a Pyrex test-tube and immerse the lower part of the tube in an oil bath, which has previously been heated to 180-185°. Stir the mixture occasionally during the first 10 minutes and push down the phthalic anhydride which sublimes on the walls into the reaction mixture with a glass rod. Leave the mixture undisturbed for 5 minutes. After 15 minutes, remove the test-tube from the bath when the liquid mass solidifies, invert the test-tube and scrape out the excess of phthalic anhydride on the walls. RecrystaUise the residue from 10 per cent ethanol or from water. 

Method 1. From ammonium chloroplatinate. Place 3 0 g. of ammonium chloroplatinate and 30 g. of A.R. sodium nitrate (1) in Pyrex beaker or porcelain casserole and heat gently at first until the rapid evolution of gas slackens, and then more strongly until a temperature of about 300° is reached. This operation occupies about 15 minutes, and there is no spattering. Maintain the fluid mass at 500-530° for 30 minutes, and allow the mixture to cool. Treat the sohd mass with 50 ml. of water. The brown precipitate of platinum oxide (PtOj.HjO) settles to the bottom. Wash it once or twice by decantation, filter througha hardened filter paper on a Gooch crucible, and wash on the filter until practically free from nitrates. Stop the washing process immediately the precipitate tends to become colloidal (2) traces of sodium nitrate do not affect the efficiency of the catalyst. Dry the oxide in a desiccator, and weigh out portions of the dried material as required. 

Place 50 g. of o-chloronitrobenzene and 75 g. of clean dry sand in a 250 ml. flask equipped with a mechanical stirrer. Heat the mixture in an oil or fusible metal bath to 215-225° and add, during 40 minutes, 50 g. of copper bronze or, better, of activated copper bronze (Section 11,50, 4) (1), Maintain the temperature at 215-225° for a further 90 minutes and stir continuously. Pour the hot mixture into a Pyrex beaker containing 125 g. of sand and stir until small lumps are formed if the reaction mixture is allowed to cool in the flask, it will set to a hard mass, which can only be removed by breaking the flask. Break up the small lumps by powdering in a mortar, and boil them for 10 minutes with two 400 ml. 

Also termed a wide-necked flask or round-bottomed flask with short ring neck (Pyrex). A tliree-necked flask may also be used and the obvious modiflcations made. 

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