Potassium iodide heat test

Analytical Methods. Most of the analytical and testing methods used for ethyl ether are conventional laboratory methods. Ethyl ether that is to be used for anesthetic purposes or in processes that involve heating or distiHation must be peroxide-free, and should pass the USP standard test with potassium iodide. This test detects approximately 0.001% peroxide as hydrogen peroxide. 

See pp 1333 under "Stability Test Heat Test with Potassium Iodide-Starch Test Stability by Heat Test at 120° or 134.5°C With Standard Methyl Violet Paper (1295—96) Stability by Surveillance Test at 65-5°C(1296) Stability by the Taliani Test for Propellants (1296-97)... 

KL) Anon, "Military Explosives", TM 9-1300-214/TO 11A-1-34 (1967). Chapter 5. Properties and Tests of High Explosives Sensitivity to Frictional Impact (pp 5 1 to 5-3) Sensitivity to Friction (5 3 to 5-6) Sensitivity to Frictional Impact (5-6) Sensitivity to Heat and Spark, which includes Explosion Temperature Test (5-6 to 5-9) Sensitivity to Initiation (5-9) Stability Tests, which include 75° International Test, 100° Heat Test, Vacuum Stability Test and Potassium Iodide—Starch Test (5 9 to 5-15) Brisance Tests which include Sand Test, Plate Dent Test and Fragmentation Test (5 15 to 5-18 and Fig 5 13 on p 5-19) Initiating Value (5-18 5-20) Sympathetic Detonation (5-20 to 5-21) Power which includes Heat of Explosion Test, Ballistic Pendulum Test and Trauzl Lead Block Test (5-21. to 5-24) Blast Effect (5-24 to 5-27) Cratering Effect (5-28 5 29) and Munroe-Neumann Effect (5-29 to 5 35)... 

The experimental conditions necessary for the preparation of a solution of a diazonium salt, diazotisation of a primary amine, are as follows. The amine is dissolved in a suitable volume of water containing 2 5-3 equivalents of hydrochloric acid (or of sulphuric acid) by the application of heat if necessary, and the solution is cooled in ice when the amine hydrochloride (or sulphate) usually crystallises. The temperature is maintained at 0-5°, an aqueous solution of sodium nitrite is added portion-wise until, after allowing 3-4 minutes for reaction, the solution gives an immediate positive test for excess of nitrous acid with an external indicator—moist potassium iodide - starch paper f ... 

Dissolve 20 g, (19 -6 ml.) of anihne in a mixture of 55 ml. of concentrated hydrochloric acid (1) and 55 ml. of water contained in a 350 ml, conical flask. Place a thermometer in the solution and immerse the flask in a bath of crushed ice (2) cool until the temperature of the stirred solution falls below 5°, Dissolve 16 g. of sodium nitrite in 75 ml. of water and chUl the solution by immersion in the ice bath add the sodium nitrite solution (3) in small volumes (2-3 ml. at a time) to the cold anihne hydrochloride solution, and keep the latter weh stirred with the thermometer. Heat is evolved by the reaction. The temperature should not be allowed to rise above 10° (add a few grams of ice to the reaction mixture if necessary) otherwise appreciable decomposition of the diazonium compound and of nitrous acid wih occur. Add the last 5 per cent, of the sodium nitrite solution more slowly (say, about 1 ml. at a time) and, after stirring for 3-4 minutes, test a drop of the solution diluted with 3-4 drops of water with potassium iodide - starch paper (4) if no immediate blue colour... 

An alternative method of removing the aniline is to add 30 ml. of concentrated sulphiu-ic acid carefully to the steam distillate, cool the solution to 0-5°, and add a concentrated solution of sodium nitrite until a drop of the reaction mixture colours potassium iodide - starch paper a deep blue instantly. As the diazotisation approaches completion, the reaction becomes slow it will therefore be necessary to test for excess of nitrous acid after an interval of 5 minutes, stirring all the wUle. About 12 g. of sodium nitrite are usually required. The diazotised solution is then heated on a boOing water bath for an hour (or until active evolution of nitrogen ceases), treated with a solution of 60 g. of sodium hydroxide in 200 ml. of water, the mixture steam-distiUed, and the quinoline isolated from the distillate by extrac-tkm with ether as above. 

While the cuprous cyanide solution is warmed gently (to 60°-70°) on the water bath, a solution of p-tolyldiazonium chloride is prepared as follows Heat 20 g. of p-toluidine with a mixture of 50 g. of concentrated hydrochloric acid and 150 c.c. of water until dissolution is complete. Immerse the solution in ice-water and stir vigorously with a glass rod so that the toluidine hydrochloride separates as far as possible in a microcrystalline form. Then cool the mixture in ice and diazotise with a solution of 16 g. of sodium nitrite in 80 c.c. of water, added until the nitrous acid test with potassium iodide-starch paper persists. The diazonium chloride solution so obtained is poured during the course of about ten minutes into the warm cuprous cyanide solution, which is meanwhile shaken frequently. After the diazo-solution has been added the reaction mixture is heated under an air condenser on the water bath fox a further quarter of an hour, and then the toluic nitrile is separated by distillation with steam (fume chamber, HCN ). The nitrile (which passes over as a yellowish oil) is extracted from the distillate with ether, the p-cresol produced as a by-product is removed by shaking the ethereal extract twice with 2 A-sodium hydroxide solution, the ether is evaporated,... 

Anon, "Military Explosives , PATR 9-1910/TO 11A-1-34(1955) Sensitivity to Impact (pp 43-7) Sensitivity to Friction (47-9) Sensitivity to Frictional Impact, which includes Rifle Bullet Impact Test (49) Sensitivity to Heat and Spark, which includes Explosion Temperature Test (49-52) Sensitivity to Initiation by Sand Test (52-3 Fig 10 on p 54) Stability Determinations, which include 75°C International Test, 100°C Heat Test, Vacuum Stability Test, and Potassium Iodide-Starch (KI)... 

The Abel heat test (heating at a temperature of 75-80°C in the presence of standard potassium iodide-starch paper). 

Heat test (Abel test). The oldest and the most popular qualitative test is the heat test introduced in Great Britain by Abel in 1865 [86]. It is called the Abel test on the Continent of Europe and the KI starch test in the U.S.A. It consists in warming a sample of nitroglycerine or nitrocellulose (or dynamite or smokeless powder) in a test tube in which a potassium iodide-starch paper moistened with aqueous glycerol solution is suspended (Fig. 1). Warming is carried out until the... 

Shorygin and Khait described the properties of nitrochitin. It bums readily when ignited. The ignition temperature is about 163°C. It withstands the heat test at 65°C for 3-8 hr (no change of the colour of starch-potassium iodide paper). 

Fit a 1-litre three-necked flask with two double surface condensers and a sealed stirrer unit. Place 25 g (29 ml, 0.25 mol) of mesityl oxide (Expt 5.213), 50 ml of dioxane and a cold (10 °C) solution of sodium hypochlorite in 750 ml of water (1) in the flask, and stir the mixture. Heat is evolved in the reaction and after about 5 minutes chloroform commences to reflux. As soon as the reaction becomes very vigorous, stop the stirrer and cool the flask with water so that the chloroform refluxes gently after 20-30 minutes, when the reaction has subsided, resume the stirring and continue it until the temperature of the mixture has fallen to that of the laboratory (2-3 hours). Decompose the slight excess of hypochlorite by the addition of sodium metabisulphite (about 1 g), i.e. until a test-portion no longer liberates iodine from potassium iodide solution. 

Heat a solution of 0.2 g of the reagent and 0.2-0.3 g of the alkene in glacial acetic acid on the steam bath for 15 minutes or until the potassium iodide test shows that the reaction is complete. Cool the mixture in ice. If a solid separates, filter it off if not, pour the reaction mixture on to 5-10 g of crushed ice. Recrystallise the resulting solid or oil from ethanol. Test Add a drop of the reaction solution to a drop of potassium iodide solution on a spot plate the presence of unreacted reagent is revealed by the liberation of iodine ... 

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