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I Norgan Ic C He Mi Str Y View Article Online / Journal Homepage / Table of Contents for this issue INORGANIC CHEMISTRY. 443 I n o r g a n ic C h e mi s t r y. Composition of Atmospheres which Extinguish Flame. By FRANKCLOWES ( PTOC. Roy. Soc., 1894, 56, 2-6) .--The experimental flame burning at a platinum jet 1 mm. in diameter, was 0.75 in. in height; it was gradually lowered into a cylinder containing the atmosphere of mixed gases, and these were considered to be in extinctive proportions if the flame was extinguished during its downward passage, or immediately on attaining its lowest position in the cylinder. The gaseous mixture was regarded as containing the minimum quantitr of extinctive gas, when the flame on being lowered into another mixture containing 1 per cent. less of such gas continued to burn in it for a few seconds before being ex- tinguished. Experiments made with flames of hydrogen and Published on 01 January 1895. Downloaded 25/10/2014 07:12:09. alcohol, varying from 0.4 in. to 1.5 in. in height, show that the varying dimensions of the flame are without influence on the proportion of carbonic anhydride in the air necessary to pro- duce extinction. Characteristic differences were observed between the behaviour of wick-fed flames and that of gas-fed flames when they were introduced into an atmosphere which extinguished them, the wick-fed flames gradually diminishing in size until they vanished, whilst the gas-fed flames gradually increased in size, becoming paler and apparently lower in temperature until they suddenly expired. The results of the experiments, of which a table is given in the original paper, show (1) that the extinction of a flame is not deter- mined simply by the proportion which the inert gas bears to the oxygen of the atmosphere into which it is introduced, but that the nature of the inert gas present also influences the result. (2) Carbonic anhydride exerts a more powerful extinctive effect on flame than nitrogen does. (3) There is a remarkable uniformity in the proportions of inert gas, which must be niixed with air in order to just extinguish wick-fed flames ; but this uniformity does not apply to the flames of combustible gases burnt from a jet. (4) The flames of gases burnt from a jet show no simple relation, as regards the proportion of oxygen present View Article Online 444 ABSTRACTS OF CHEMICAL PAPERS, in the extinctive atmosphere, tJothe relative proportions of oxygen re- quired for their complete combustion. In the presence of the hydrogen flanie carbonic anhydride does not suffer partial deoxidation. The introduction of a minimum of 15 per cent. of carbonic anhydride into air is necessary to cause it to extinguish ordinary wick-fed flames. For the extinction of coal-gas flames, however, the addition of 33 per cent. of carbonic anhydride is necessary, and for the hydrogen flanie 58 per cent. E. C. R. Preparation of Perchloric acid and its Use in the Esti- mation of Potassium. By D. ALBERTKREIDEE (Zeit. anorg. (!hem., 1895, 9, 342-348).-Sodi nm chlorate is converted into pef- chlorate by cautiously heating during 1;-2 hours, the residue being dissolved in water, and hydrochloric acid added in quantity suficient to decompose any unaltered chlorate ; the solution is then evaporated to dryness, stirring vigorously towards the end of the operation, as otherwise the perchlorate retains some water and solidifies so that it cannot be removed from the dish. The finely pulverised residue is treated with concentrated hydrochloric acid, filtered from the sodium chloride, and well washed with hydrochloric acid, which is then re- moved from the solution by evaporation. The perchloric acid is sufficiently pure for the determination of potassium, for the slight residue obtained when it is evaporated is completely soluble in alcohol (97 per cent.), and consists of sodium perchlorate. If the sodium chlorate contained potassium chlorate the pulverised crystals of chloride and perch!orate are treated with alcohol (97 per cent.), which dissolves the latter more readily than the former, the alcohol is removed, and the residue treated with hydrochloric acid as above. The solubility of sodium perchlorate in alcohol (97 per cent.) is 0.2 grain per C.C. The preparation of perchloric acid, including the separation of the potassium salts, occupies about two days ; 100-300 Published on 01 January 1895. Downloaded 25/10/2014 07:12:09. grams of sodium chlorate may be conveniently employed. For the estimation of potassium, the substance, which must be free from snl- phuric acid, is dissolved in hot water (20 c.c.), perchloric acid (1.5 times the theoretical quantity) added, and the solution evaporated to a SSrup, stirring constantly. It is then again dissolved in water and evaporated, the residue being washed twice with about 20 C.C. of 97 per cent. alcohol containing 0.2 per cent. of perchloric acid, the alcohol is decanted through an asbestos filter, the crystals dissolved in hot water (10 c.c.) containing a little perchloric acid, and the solutioii again evaporated to dryness ; the residue is finally washed on to the filter with the smallest possible quantity of the alcoholic perchloric acid, treated once with pure alcohol, dried at 130°, and weighed. The alcoholic washings shotild not exceed 50-70 C.C. The removal of phosphoric acid is unnecessary, but if if is present the potassium perchlorate should remain in contact with perchloric acid. iii excess, before treating with alcohol. The analytical results are satisfactory. J. B. T. Density of Nitrogen. By LORDRAYLEIGH (Proc. Roy. XOC.,1894, 55, 340-344) .-In a previous paper (€'roc. Roy. SOC.,53, 146), the View Article Online INORGANIO OHEMISTRY. 445 author has shown that nitrogen prepare‘d by Lupton’s method is lighter, by about 1/1000 part, than that derived from air in the usual way. It is now shown that nitrogen derived entirely from chemical compounds is materially lighter than atmospheric nitrogen. This difference amounts to about 1/200 part of the whole. Mean density. Nitrogen from nitric oxide by hot iron.. .. .. 2.30008 Nitrogen from nitrous oxide by hot iron . .. .. 2.29904 Nitrogen from ammonium nitrite by hot iron . .. 2.29869 Atmospheric nitrogen by hot copper (1892) .. ,. .. 2.31026 Atmospheric nitrogen by hot iron (1893). .. 2.51003 Atmospheric nitrogen by ferrous hydrate (1894). 2.31020 Experiments have proved that the densities do not alter when the gas is exposed to the Bilent electric discharge. The author demon- strates that the lightness of the nitrogen from chemical compounds cannot be due to the presence of impurities such as hydrogen, ammonia, water vapour, &c. J. J. S. Reduction of Nitric Oxide by Moist Iron or Zinc. By PAUL SABATIER and J. B. SENDERENS (Compt. rend., 1895,120,1158- 1161).-Nitric oxide in contact with moist zinc turnings over water is at first reduced to a mixture of nitrous oxide and nitrogen with a, small quantity of hydrogen. If the action is allowed to continue, the proportion of nitrous oxide diminishes, whilst that of nitrogen and hydrogen increases, the gas finally being a mixture of nitrogen and hydrogen only. The hydrogen is doubtless a result of the action of the ammonia on the zinc. In contact with moist iron, standing over mercury, the nitric oxide is reduced to a mixture of nitrous oxide and nitrogen, in the pro- portion of 2 vols. of the former and 1 rol. of the latter, with a Published on 01 January 1895. Downloaded 25/10/2014 07:12:09. small quantity of hydrogen, which results most probably from the action of the iron on the water in presence of mercury. The reduction of the nitric oxide takes place slowly, probably because of its slight solubility in water. A solution of the gas in ferrous sulphate solution is much more rapidly reduced, and the gas produced consists at first of 2 vols. of nitrous oxide with 1vol. of nitrogen, but after a the the proportion of nitrous oxide diminishes and that of nitrogen increases, whilst hydrogen is also given off in gradually increasing proportion, until at the end of the action the gas is a mixture of nitrogen and hydrogen only in practi- cally equal volumes. The iron becomes covered with hydrated ferroso- ferric oxide. Similar result8 are obtained with zinc. C. H. B. New Polyphosphoric Acid, H,P,O,,, and its Salts. By FRITZ SCHWARZ(Zeit. awry. Chem., 1895, 9, 249-266) .-Salts of tetraphos- phoric acid have been described by Fleitmann and Henneberg (Anna- Zen, 65,322), the sodium salt being obtained by melting the anhydrous pyrophospliate with hexametaphosphate. It crystallises with 36H20. Fleitmann and Henneberg’s acid tetraphosphate, Na4H2P40,,,is formed from the salt Na,H2P207by the removal of the water of crystalli- sation. VOL. Lxvm. ii. 34 View Article Online 446 ABSTRAOTS OF CHEMIOAL PAPERS. Sodium triphosphate is best obtained by melting 100 grams of the pyTophosphate with 50-55 grams of metaphosphate ; after keeping it in a fused state for about 15 minutes, it is allowed to cool slowly, and the product is broken into small pieces and cautiously dissolved in cold water. The solution, allowed to remain all nigbt, is filtered, and the filtrate evaporated spontaneously ; the crystals which are deposited can be recrystallised from cold water, but great care is necessary, as the heat developed on treating them with water is sufficient to partially convert the salt into metaphosphate. It crystal- lises from water with 16H20 in transparent crusts, loses water on exposure to air, and is very soluble. The solution has a faintly alka- lirie reaction; when boiled, it is quickly converted into pyrophos- pbate, whilst with mineral acids and some organic acids it yields pyrophosphate in the cold, and also orthophosphate when heated with them.
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