Casserole

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. 

Method 2. From chloroplatinic acid. Dissolve 3 - 5 g. of the purest commercial chloroplatinic acid (3) in 10 ml. of water contained in a 250 ml. P3rrex beaker or porcelain casserole, and add 35 g. of A.R. sodium nitrate (1), Evaporate the mixture to dryness by heating gently over a Bunsen flame whilst stirring with a glass rod. Then raise the temperature... 

Carry out this preparation in the fume cupboard. Dissolve 100 g. of chloroacetic acid (Section 111,125), contained in a large porcelain basin or casserole, in 200 ml. of water. Warm the solution to about 50°, using a 200° thermometer as a stirring rod. Introduce 90 g. of pure, powdered sodium bicarbonate in small quantities at a time with stirring maintain the temperature at 50-60° until effervescence ceases. Now add 80 g. of pure, finely-powdered potassium cyanide (or an equivalent quantity of sodium cyanide), stir the mixture without further warming until the... 

To obtain catalyst of maximum and reproducible activity, it is recommended that the fusion be conducted in a Pyrex beaker or casserole resting in a cavity of a copper block heated with a burner and provided with a thermometer well. Adequate temperature control is thus possible. Short, J. Soc. Chem. Ind. 55, 14T (1936). 

Ammonium chloroplatinate often can be used to advantage in place of chloroplatim c acid in the preparation of Adams catalyst. A mixture of 3 g. of ammonium chloroplatinate and 30 g. of sodium nitrate in a casserole or Pyrex beaker is heated gently at first until the rapid evolution of gas slackens and then more strongly until a temperature of 500° is reached. This operation requires about fifteen minutes and there is no spattering. The temperature is held at 500-520° for one-half hour and the mixture is then allowed to cool. The platinum oxide catalyst, collected in the usual way by extracting the soluble salts with water, weighs 1.5 g. and it is comparable in appearance and in activity to the material prepared from chloroplatinic acid. 

Hengst, m. stallion jack (Br ictnj ) old piece. Henkel, m. handle, lug, ear. -schale, /. casserole. 

If the fusion temperature is about 300°, the yield of platinum oxide is very low, at higher temperatures the yield increases, and at temperatures of 450° and higher it is practically quantitative. With a proper fusion a slightly lower yield than quantitative is generally not due to non-precipitation of the platinum but to loss by spattering and to deposition of a small amount on the casserole. 

Quantitative analyses show the oxide to be Pt02. H20.a i It usually contains a very small amount of glaze from the casserole, but this does not affect its Use or activity. The oxide... 

The thin film of oxide which remains in the casserole is dissolved by treating with a little constant-boiling hydrobromic acid (Note 7) the solution obtained may then be evaporated and the residue added to the next fusion mixture. 

Porcelain apparatus. Porcelain is generally employed for operations in which hot liquids are to remain in contact with the vessel for prolonged periods. It is usually considered to be more resistant to solutions, particularly alkaline solutions, than glass, although this will depend primarily upon the quality of the glaze. Shallow porcelain basins with lips are employed for evaporations. Casseroles are lipped, flat-bottomed porcelain dishes provided with handles they are more convenient to use than dishes. 

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Collect filtrate in a 250 Erlenmeyer flask. Cool to RT and add 2ml of 0.1M K chromate indicator to the filtrate. (For the prepn of 0.1 M K chromate see 4.4.3.S.3). Titrate to the end point with 0.1N Ag nitrate. (For the prepn of 0.1N Ag nitrate soln, see 4.4.3.5.4). The end point is noted by the first of a permanent colored red ppt of Ag chromate. The end point should be detd by using a white background or by transferring filtrate plus a minimum of distd w washings to a white casserole... 

When detn of yield is required, use a, large sample of glycerol (about lOOg) and Method No 1, which is conducted in an open lead casserole of about 1 liter capacity using for an agitator a thermometer inserted in a lead pipe with a slot for reading... 

Place the nitraror (lead casserole of 1 liter capacity) into a large earthenware dish contg a cooling mixture of ice and large Crystals of common salt... 

Note If the temp rises above 15°, stop adding the glycerol. If the rise in temp is fast with evolution of copious brownish-red fumes, drown the mixture in at least 5 liters of water io a beaker or casserole. Never dump into the sink... 

Fuse ca 100 g of pure resorcin in a porcelain casserole and immediately pour on a Pyrex glass plate. Cool and grind the cake in a mortar to pass a US Standard No 6 mesh screen. Pour 400 g of 98% nitric acid into a pint size Dewar jar and add, In small portions, while mechanically stirring, snow of carbon dioxide, until the temperature drops to -20°C. Add, in small portions and with... 

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