analytical chemistry. - ACS Publications


analytical chemistry. - ACS Publicationspubs.acs.org/doi/pdf/10.1021/ja02012a022Of the total bituminous content, one-fif...

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Review of A m erica n ChemicaI Research,

Asphalt Rock in Kentucky. BY W.E. BROCK. E ? g . Mii7i. 2 7 , 1903 ( , f r o m a&. sheets oy :Winei*al IudustYy).-The " black-rock ' ' strata coiitairi u p to 4 per cent. of bituminous matter, and are of no commercial value, :he interveiling asphaltic strata are j to I j feet i n thickiiess and coiitairi j to 15 per cent. Of the total bituminous content, one-fifth is asphaltene and fourfifths petrolene. After the bitumen is extracted, the sandstone which it impregnated falls to a very fine powder. Only tile deposits near the railways are being worked. For street coniposition, the rock is crnshed a t or near the quarries, and mixed. when used, with pulverized limestone or marl aiid an asphaltic cement composed of Trinidad gum asphalt or petroleum residue. Details are given respecting the various deposits. T h e value of the outJ . 11'. R r c I r A R m . put i n 1902 was $68,704.

3.,June

ANALYTICAL CHEMISTRY. Refractometers and Some of Their Uses in Analytical Chemistry. BY W. F. EDWARDS. PYOC. Colo. Sci. SOC., 7 , 85-102 ; figures-Devoid of original matter. T h e author regards it as very unfortunate that arbitrary scale instruments are in use in the case of fixed oils and fats. H e wishes that instrument makers would furnish them with tables whereby the readings could be used to find the iiidex of refraction, and that investigators would use these tables instead of publishing arbitrary numbers. W.F. HILLEBRAND. Report of the Committee Appointed by the Ohio Gas Light Association to Determine Standard Methods of Testing Fuel Gas Appliances. Anter. Gas Light /., 78, 84~-88g.-The committee, Messrs. H. L. Doherty, F. W. Stone, and John Franklin, give rigid methods for determining the efficiency of instantaneous and illdependent water heaters, and of the top-burners, ovens, and broilers of gas-ranges. All of these appliances are made to heat water flowing at such a rate as to be discharged a t a fixed temperature. T h e conditions under which this is to be done for each appliance and the apparatus for it are given in much detail. T h e efficiency is to be determined for varying rates of consumptiori of the gas ; it is to be stated in per cent., and is determined by dividing the total heat added to the water by the total heat the gas is capable of developing. This last quantity is to be determiiied by calorinietric measurement or by calculation. T h e losses are due in all cases to radiation and to the sensible heat carried off by the products of combustion, this being divided into necessary loss and that due to over-ventilation. I n the case of ovens, the committee adds t h e loss due to incomplete combustion, which may be determined by analysis of the products of combustion. T h e losses due to sensible heat carried off are deteriniued

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by multiplying the rise in temperature of the flue gases by the quantity of each constituent and its specific heat, and then adding these products together. For making the flue-gas analysis, the committee recommends the Orsat apparatus. (This recommendation seems unfortunate to the reviewer, because in the Orsat apparatus oxygen can be completely removed only by passing the gas to he analyzed a great number of times back a‘nd forth between burette and absorption bulb. T h e point of complete removal is very difficult to observe, because the decrease in volume after each absorption, except the first few, is very slight. All of the oxygen that is not removed by the alkaline pyrogallol is absorbed by the cuprous chloride solution and thus appears in the analysis as carbon monoxide.) T h e necessary heat loss is obtained by calculation, and the difference between this value and the one found for the total heat lost through the products of combustion gives the loss due to over-ventilation. T h e loss due to radiation should be represented by the difference between the total heat the gas is capable of developing and the sum of the heat added to the water and that carried off by the products of combustion. I n the case of ovens, the committee would determine the radiation by finding the length of time it takes to melt enough ice in the oven a t room temperature to yield two pounds of water, An alternative in determining the efficiency of the topburner is to find how much water i t will cause to evaporate in a given time with varying rates of gas consumption. BENTONDALES. A System of Qualitative Analysis, Including Nearly All the Iletallic Elements. Introduction. Part I. Preparation of the Solution. BY A. A. NOYES. Technology Quarter&, 16,93-131. -This is a preliminary publication of an investigation which has been carried on during the past three years by Professor Noyes and a number of co-workers. T h e work is being pursued on a broad and strictly experimental basis and promises to be by far the most notable contribution to qualitative analysis that has appeared for many years. T h e scope and plan of the undertaking is indicated in the following quotations from the introduction : T h e aim of this investigation has been to work out in detail a systematic, universally applicable scheme of qualitative analysis which shall include as nearly as practicable all the metallic elements, and which shall make possible their detection even when present in quantities as small as I or 2 milligrams.” “The system of analysis will be primarily divided into a series of parts: Part I will treat of t h e preparation of the solution; Part I1 of the analysis of the tungsten and niobium groups : Part I11 of the analysis of the selenium and silver groups ; Part IV of the analysis of the platinum group and the detection of lead and tellurium ; Part V of the analysis of the ruthenium, iridium, copper,

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and inolybdenum groups ; and the succeeding parts, of the rare earth, aluminum and iron, alkaline earth, and the alkali groups. Under each part is first presented a tabular outline which will give a survey of the important steps and the chemical reactions involved in the procedure. This is followed by a general discussion in which are presented the reasons for the adoption of the process employed. Then comes the procedure itself, and the explaiiatory notes upon it. Next are presented confirmatory experiments and references, which serve to substantiate the statements made in the notes and to justify the details of the procedure. Finally are given the test analyses, which were made with known mixtures according to the procedure, in order to test its efficiency. ’ ’ In Part I, which forms the subject of the article, radical departures are made from the ordinary course of procedure in the preparation of solutions for the detection of the metals. T h e paper is so replete with details that it can hardly be given in abstract. THEODORE WHITTLESEY. A Study of the Quantitative Determination of Antimony, BY LEWISA. YOUTZ. School ojMincs Quavf., 24, 13j-144.-The work here described was undertaken with the hope of finding a method of separation of tin from antimony, analogous to Fischer’s method of separating arsenic chloride by distillation. Stannous chloride dissolved in aqueous hydrochloric acid does not volatilize, except in traces, at the boiling-point of the solution, even when the boiling-point is raised to 150’ by adding zinc chloride. Stannic chloride volatilizes slowly and partially from a solution containing zinc chloride above 1 2 j o , in a stream of hydrogen chloride, Antimony trichloride behaves similarly under t h e same conditions, the volatilization becoming appreciable at a slightly lower temperature. Solutions of antimony salts oxidized with either nitric acid or potassium chlorate are not volatile a t 145’. No analytical separation of antimony and tin could be effected H. N. McCoy. by distillation.

Notes on the Ammonium Molybdate Precipitation of Phosphorus. BY J. W. BEATTY. Iron Age, May 28, ~gog.-Precipitations mere made in different menstrua, viz., nitric acid, hydrochloric acid, ammonium nitrate with free nitric acid, ammonium chloride with free nitric acid, and ammonium chloride with free hydrochloric acid. T h e results were all satisfactory ; the only differences were the longer time necessary for settling of the precipitate when using hydrochloric acid. An ammonium molybdate solution was made u p with hydrochloric acid instead of with the usual nitric acid, and precipitations were likewise satisfactory in either nitric acid or hydrochloric acid solutions, except that longer time was necessary for complete settling in the bottom. J. \v. RICHrlRDS.

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Loss of Sulphur in Pig-Iron Borings. BY W. E. DICKSON. A g e , June 1 1 , 1903. (Read before the American Foundrymen's Association.) T h e discovery was made that carefully kept borings lost sulphur on standing, some very old samples having lost as much as 40 per cent. of their total sulphur content. T h e loss is probably due to slow oxidation. Steel standards show no loss, possibly due to their rolling u p into compact lumps which present little porous surface. J. W. RICHARDS.

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Electrochemical Analysis : Determination of Lead as Dioxide. BY I. MOLTKEHANSEN.Elecfrochemical hzdusf?y, June, rgo?.-The writer made tests to find the exact quantity of free nitric acid which should be in solution to separate lead from manganese satisfactorily, and the limits o i accuracy of t h e method. By using high current density, strong acid, and a hot electrolyte, the manganese is kept in solution as permanganic acid, while lead is precipitated on the anode as PbO,. There must be less than I Mn to 2 Pb to get a clean separation, but the method would appear to be useful in many cases, such as analyzing galena. With less than 0.03 gram Mn present, and over 0 . I gram Pb, the electrolyte should contain 2 j to 27 cc. of nitric acid (sp. gr. 1 . 4 2 ) to I jo cc., corresponding to 18 per cent. pure HNO, ; electrolysis is started a t 70' C., with z amperes to 1 5 0 sq. cm. anode area. If as much as 0.04 gram Mn is present, eithermore HNO, is added, say 35 cc. of 1.42 acid, or else 25 to 27 cc. is added a s before and a few cubic centimeters of oxalic acid solution are added as soon as flakes of manganese hydroxide form in the electrolyte. T h e analysis takes thirty-five to fifty minutes. T h e anode is washed well with water, dried, and weighed. No lead conies down on the cathode as long as the amounts of nitric acid mentioned are added. J. W. RICHARDS.

On the Present Status of the X-Rays. Use in Qualitative Analysis. BY M. I. WILBERT. 1. Fvankli?z Insf., June, 1903.X - r a y s h a w been found of considerable use in detecting adulterations of inorganic materials in drugs or chemicals of organic origin ; drugs like the gums, gum resins aud resins are rather difficult to examine in the ordinary way, but may be readily tested by these rays. I n coal, asphalt and other materials of a like character, the amount as well as the distribution of the ash or inorganic material may be readily determined. In cases of medical and surgical treatment, the use of these rays has more than come u p to the expectations, and bids fair to be of even more use ; the technical and applied scientific purposes for which they are suitable have not been so thoroughly exploited as they J. W. RICHARDS. deserve. The Commercial Assay of Lead Ores. BY A. W. WARWICK. Proc. Colo. Sci. Soc., 7, 109-1I I .-The author defends against at-

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tack the position assumed by him a t an earlier date (this Journal, 25, R 2 j 4 ) and offers further evidence to prove that the fire assay for lead gives much lower results than the wet assay, especially on poor ores. See also in this connectioii this Journal, 25, R 122.

TIr. F.

HILLEBRAND.

ilETALLUROICAL CHEIllSTRY AND ASSAYING. Louisiana Purchase Exhibition : iletallurgical Exhibits. Iron nizd Mach. World, May 16, IgOg.--The general article of sixteen pages describes the exhibition in detail, with fine illustrations. Director Skiff writes on Exhibits at f h e Expositioii, H. T. Rogers on Exhibits of Technical Schools, J . Ockersoti oti Civil, Military and Architectural Exhibits, T. 31,Moore 0x1 the Depavtnzeizt of Machiizerq,, W. E. Goldsborough on the Deparfmeizt of Electricib, 1x1. A. Smith on Tva?zsportafio?z E x h i b i t s , and J. A . Holmes on Minizg aizd ,4fefallzwgical E x h i b i f s . Many of t h e modern metallurgical processes will be shown in actual operation, and some of the most primitive apparatus also, such as the Mexican .4wastra. J . W .RICHARDS. Industrial Pittsburg. BY Vi-, G. IRWIN.Recent Growth of Cincinnati. BY R. H. SHERWOOD. Ivoiz a i d Mach. LVodd, May 16, 1go3.-A timely r6sum6 of tlie resources and productiveiiess of these districts, in the various metallurgical and allied J. \Ir. RICHARDS. in d 11s t ri e s . On the Industrial Importance of Metallography. BY A. S A U V E U R . 1, Fraizkliit Inst., April, 1903.--A lecture confined to the metallography of iron and steel. Cast iron is to be regarded as very high carbon steel plus a certain nmouiit of graphitic carbon. T h e close relation between structure, treatment and properties cannot be detected by chemical analysis, but only by microscopy; it is of as great importance to impart the right structrire to a metal as to secure for it a desirable composition, Mr. Kreuzpointtier, in the discussion, thought that it would be some time yet before we could tell tlie working qualities of a steel simply by the niicroscope. Mr. G. H . Claxner has made considerab!e use of this new method of investigation 011 other metals than iroii and heartily endorses Saureur’s statements a s to its pracJ. IT.RICHARDS. tical importance. A Modern Method of Coal Washing. BY C. A. MEISSNER. B7ig. Mi7z. /., May 9, 1903 (paper before Nova Scotia Mining Society) .-Descriptive of an apparatus which can be applied t o concentrating ores a s well a s to washing coal. T h e specific gravity of pure coal is 1.0 to 1.3, of slate 2 to 2 . 7 , pyrites 3.1 to j.1. Successful action is entirely dependent 011 uniformity of size. T h e coal is passed through a grizzly to ’/* inch, and then passed from a hopper into a chute, where it is washed onto the beds by a