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An Aly Tical Chemistry View Article Online / Journal Homepage / Table of Contents for this issue 698 ABSTRACTS OF CHEMICAL PAPERS. Published on 01 January 1909. Downloaded 24/10/2014 13:06:11. An aly tical Chemistry . Analysis of Coal-Gas and Similar Gaseous Mixtures ; Estimation of Nitrogen in Coal-Gas. GEORGVON KNORRE(Chem. Zeit., 1909, 33, 717--719).-The first part of the paper consists in a criticism of the methods usually employed in analysing coal-gas, Jager's process (partial cornbustion with copper oxide) may be improved by first expelling the air from the small combustion tube by means of nitrogen, which may be readily made for the purpose by introducing air into the phosphorus pipette. The combustion tube is best made of fused silica. If nitrogen only is to be estimated, 100 C.C. of the coal-gas are at once passed slowly over the red-hot copper oxide. L. DE K. View Article Online ANALYTICAL CHEMISTRY. 699 Reduction of Perchlorates by Titanium Sesquisulphate. ARTHURSTAHLER (Chem. Zeit., 1909, 33, 759).--h criticism of Rothmund’s process (this vol., ii, 434). The author has used titanium sesquisulphate for the reduction of perchlorates previously (Ber., 1903, 36, 166, 1549), but the results (titration of the excess of the sesqui- sulphate with iron solution) were not very satisfactory. Good results, however, may be obtained by estimating the chloride formed in the reaction as proposed by Rothmund. For small quantities of chlorine, Richard’s nephelometer (Abstr., 1904, ii, 287) is recommended. L, DE K. Estimation of Iodine in Protein Combinations. LOUISW. RIGGS(J. Arner. Chem. Soc., 1909, 31, 710-717).-1n the estimation of the iodine in protein combinations by Baumann’s method (Abstr., 1896, ii, 487), a portion of the halogen is oxidised to iodate during the fusion. After the estimation of the iodine,.present as iodide, by the usual method, it is necessary, particularly in the case of proteins of small iodine content, to reduce the iodate by Devarda’s alloy and sodium hydroxide, and to estimate the iodine in the iodide thus formed. Mixtures of protein substances and. potassium iodide, analysed by the foregoing process, do not give results comparable with those obtained by the analysis of a protein substance containing combined iodine. Excess of nitrous acid reduces iodates in sdch a way that the iodine cannot be estimated colorirnetrically in carbon tetrachloride. C. S. Estimation of Sulphur in Coals and Cokes. M. HOLLIGER (Zeitsch. angew. Chem., 1909, 22, 1361--1362).-A reply to Dennstedt (compare this vol., ii, 343,435). The author thinks Dennstedt’s process a good one, but advises the use of a small Peligot tube filled with hypobromite solution as a trap. The contents are afterwards tested Published on 01 January 1909. Downloaded 24/10/2014 13:06:11. for sulphuric acid, L. DE K. Estimation of Total Nitrogen by E. A. Mitscherlich’sMethod. VINCENTSCHENKE (Chern. Zed., 1909, 33, 712-713).--8 reply to Mitscherlich and Herz and Mitscherlich and Merres (this vol., ii, 614). The author prefers his own process (Chem. Zeit., 1896,20, 1032, 1033). The following process is recommended in the presence of any appreci- able amount of nitrites : 0.5-2 grams of the substance, and so much potassium chlorate that there is one part of this to three parts of nitrous acid, are placed in a round-bottomed flask, 50 C.C. of water are added, and then drop by drop 3 C.C. of dilute sulphuric acid (1 : 2). After a quarter of an hour, 2-4 grams of reduced iron are added, and then 15 C.C. of the dilute acid (Ulsch’s process), and when the reduc- tion of the nitrate to ammonia is accomplished, the organic substances are destroyed by evaporating with 30 C.C. of sulphuric acid and a few drops of mercury (Ejeldahl method). A blank experiment should be made, once for all, to test the purity of the reagents used. 1,. DE K. Detection of Nitrates in the Presence of Bromides. VILLEDIEC (J. Pharm. China., 1909, 30, 66--67).-When testing for nitrates in View Article Online 700 ABSTRACTS OF CHEMICAL PAPERS. the presence of a largebexcess of bromides, it is advisable to remove the latter; this can, of course, be effected with silver sulphate, but in practice this is rather inconvenient on account of its slight solubility. The following test is recommended. The liquid, neutralised if necessary, is mixed with a slight excess of basic lead acetate, which precipitates nearly all the bromine, and the filtrate is then heated to boiling and the excess of lead precipitated by adding a little powdered sodium sulphate. To the filtrate the usual test for nitrates with ferrous sulphate and sulphuric acid is then applied. L. DE K. Estimation of Phosphorus in Urine. G.C. MATHISON(Bio-Chem. J., 1909,4,233-239).-The estimation of total phosphorus in urine is best carried out by Plimmer and Bayliss’s modification of Neumann’s method ; and inorganic phosphates by precipitation with magnesium citrate mixture, incineration, and calculation from the weight of the ash .(Mg2P207). Magnesia mixture gives incorrect results, owing to partial precipitation of calcium and of organic phosphorus, Organic phosphoric acid is determined by subtracting the inorganic from the total phosphoric acid, or by applying Neumann’s method after the removal of inorganic phosphates. The uranium acetate method is inaccurate. Organic phosphorus must be estimated while the urine is fresh, as it decomposes in stale urine, especially if ammonia is present. It is readily dialysable. W. D. H. Disappearance of Arsenic in the Form of Gaseous or Volatile Compounds during Putrefaction. MARIOTONEGUTTI (Boll. Chim. Farm., 1909, 48, 259-264, 370-374). -The author’s experiments show that the putrefaction of protein substances contain- ing arsenic is not accompanied by the evolution of arsenical gases, Published on 01 January 1909. Downloaded 24/10/2014 13:06:11. although very small proportions of organic arsenical products having basic or ptomaine characters are formed, which are volatile at a temperature above 30°, probably between 50’ and 60”. The dis- appearance of arsenic from corpses in the form Df gaseous compounds is hence improbable. 1’. H. J?. Gravimetric Estimation of Boric Acid. KURTARNDT (Chem. Zed.,1909,33,725-726). -The process is intended for the estimation of small qiiantities of boric acid in fused alumina ; 15 grams of potassium hydroxide are fused in a nickel crucible until the mass runs quietly, and, when cold, 3 grams of the impalpable powder are sprinkled over the surface. The mass is now again heated to redness for three hours, the crucible being covered. When cold, the contents are dissolved in water, slight excess of siilphuric acid is added, and the solution is introduced into a Gooch goose-neck apparatus. The authors have slightly modified this apparatus so that it holds fully 150 C.C. The boric acid is then expelled by repeated distillation with methyl alcohol, the distillate is evaporated, as directed by Gooch and Jones (Abstr., 1899, ii, 331), with a known weight of sodium tungstate, and the residue ignited and weighed. When a solution of alumina and boric acid is mixed with ammonia, View Article Online ANALYTICAL CHEMISTRY. ’101 a portion of the acid is retained obstinately by the precipitated hydroxide. L. DE I(. Estimation of Boric Acid. R. MANDELBAUM(Zeitsch. ano~g. Chem., 1909, 62, 364-369). -The distillation of boric acid with methyl alcohol (Spindler, Abstr., 1905, ii, 480) may be used as an accurate method of estimation when modified. The borate, or substance containing borates, is warmed with 40% phosphoric acid, any carbon dioxide formed expelled by a current of purified air, the flask connected with a condenser, and a receiver containing a known excess of standard sodium hydroxide attached. Absolute methyl alcohol (150-170 C.C. for 0.2 gram B,OJ is run into the flask, which is then heated, a current of air saturated with methyl alcohol being bubbled through it. Finally, the sodium hydroxide flask is warmed to expel methyl alcohol, which distils through a second condensar into a receiver. The sodium hydroxide is then cooled, mixed with half its volume of glycerol, and titrated with sulphuric acid, phenolphthalein being used as indicator. The analysis occupies two to three hours. C. H. D. Elementary Analysis According to Carrasco-Plancher. ORESTECARRASCO (Chsm. Zeit., 1909, 33, 733-734, 755-756).-An improvement of the apparatus described previously (Abstr., 1896, ii, 201). The copper oxide has been replaced by ‘‘platinum biscuit,” and different combustion tubes are used according to the nature of the substauce (solid, liquid, readily volatile, etc). Nitrogen-, sulphur-, and halogen-containing substances may also be analysed by means of the apparatus. L. DE K. Simultaneous Estimation of the Residue and Combined Published on 01 January 1909. Downloaded 24/10/2014 13:06:11. Carbon Dioxide in Waters. K. CHARITSCHKOFF(Chem. Zeit., 1909, 33, 670)-A slight modification of the Rohrbeck-Geissler apparatus for the estimation of carbon dioxide in carbonates from the loss sustained on adding hydrochloric acid. The lower, basin-shaped, part of the apparatus may be removed and weighed, and serves for estimating the residue of the water in the ordinary way. The upper part of the apparatus is then put on, and the carbon dioxide is estimated as usual. L. DE K. Estimation of the Alkalinity of Bleaching Powder Solu- tions. KENNEDYP. ORTON and W. J. JONES(Analyst, 1909, 34, 317-318).--8 known volume of the solution is added to an excess of N/lO-hydrochloric acid contained in a Drechsel bubbler, and a rapid current of pure air is drawn through for forty- five minutes, the solution being i meanwhile carefully shielded from light.
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