Search Documents

Jan 1, 1942

By W. P. Blake

Forty-five years have passed since I discovered the extensive and remarkable diatom-earth beds at Monterey, California., and now I have the satisfaction of bringing to notice still another wonderful deposit in the heart of Arizona. The Monterey beds mere described at the Philadelphia Academy,* and specimens were sent to Prof. J. W. Bailey, West Point, N. Y., at that time the leading American authority upon such microscopic relics of organic life. The earth from both localities is snow-white and pulverulent. It rubs off' like soft chalk upon the fingers when handled, and has the general appearance of chalk. But, unlike the Monterey beds, these newly-discovered deposits consist largely of volcanic ash, through which the siliceous shells of the diatoms are distributed. These deposits are in the central portion of the San Pedro valley,† in the southeastern corner of Pinal county. The region of their greatest development is a few miles south of the mining town of Mammoth, on the east bank of the stream, and near Redington, some 40 m. N. of Benson, on the Southern Pacific railway. The altitude is about 2600 ft. above tide. This portion of the San Pedro valley lies between the high Catalina and Rincon ranges on the west and the Galiuro mts. on the east. The Catalinas are composed chiefly of crystalline DIRECTOR OF THE ARIZONA SCHOOL OF WINES,

Jan 1, 1903

Mr. Cottrell : I omitted to speak of the cost of installation. The precipitation-plant at the Balaklala smelter, up to the time of initial operation, including the construction of flues, installation of the apparatus, etc., cost $107,000, and subsequent modifications probably represented at least $15,000 more. Upon the information gained in this plant, the installation at the cement-mill, handling nearly twice as much gas, has been reduced in cost in a number of ways, but the overhead construction, carrying the precipitator at the top of the stacks, is naturally expensive, yet, even so, the total cost of construction will probably not greatly exceed $150,000. The mechanical details of the tubular form last shown have been worked out more recently than those of the plate form, and the tubular form promises to be still less expensive in construction, as you would naturally expect. The cost of operat-ing the plant varies somewhat with the character of the gases used. The amount of power consumed is not determined by the tonnage of the material collected, but by the volume of gas to be handled. It takes as much power to precipitate a thin cloud as a dense one. In the cement-plant they are getting a higher efficiency; i. e., a greater number of cubic feet treated per kilowatt than in the earlier plants. This is perhaps partly due to higher temperature of the gases, which here average about 450° C. The best figures on the cement-plant are between 3 kw. and 4 kw. Of

Jan 1, 1913

By E. W. Parker

PROBABLY everyone is well aware that from April 1 to September 11, 1922, anthracite production was completely suspended; during those 163 days not one ton of coal was produced in the anthracite region. The production loss was about 30 million tons, and although production is now at its peak, there is no possible way by. which, within any short space of time, that deficiency can be made up. During that time the miners sacrificed in wages something over 100 million dollars. The anthracite companies paid out in cash, keeping their mines in condition to operate when mining should be resumed, something like 30 million dollars without taking in one cent of revenue. The tonnage of domestic sizes included in that lost output was about 21 million tons. The anthracite operators figured that between September 11, 1922, and March 31, 1923, they would possibly be able to produce about 60 per cent. of the tonnage that was mined the preceding year, that is, from April 1, 1921, to March 31, 1922. The problem then arose as to how that tonnage could be distributed equitably throughout the United States and Canada. We had in our records in Phila-delphia the distribution by communities, about 20,000 of them, to which anthracite had been shipped during the last five years, so that we were well posted as to what each community should be entitled to receive. We allotted to each of those 20,000 communities 60 per cent. of the tonnage that it had received during the preceding coal year, and we have endeavored to see that whatever tonnage we have been able to produce should be equitably distributed on that basis. It was a matter simply of voluntary cooperation by the anthra-cite operators who placed the distribution of their tonnage practically in the hands of the Pennsylvania Fuel Commission; the anthracite companies have almost without exception acceded to every request that we have made of them. When communities were reported entirely out of coal, a telegram or letter to the directors obligated to that community has resulted in some anthracite being shipped there, so that we have thus far kept the distribution on a fairly equitable basis. Prior to the suspension of mining operations, pre-liminary negotiations were carried on for the renewal of the wage scale, the operators thinking that it could be adjusted satisfactorily, and that the same method of procedure would be followed as during the 20 years succeeding the strike of 1902. At every termination of the wage agreement since that date, until last year, an agreement had been reached early in the season that mining operations should be continued, with the under-standing that any new agreement should be retroactive to April 1. At the meeting of the committees of anthra-cite operators and miners, on March 21, 1922, the opera-tors were presented with an ultimatum by the miners to the effect that unless an agreement were reached within ten days, mining operations would cease. That was protested against by the committee of operators as being unfair, not only to the operators and the public but to the men themselves. In spite of this protest the suspension occurred and, as you know, continued until September 11.

Jan 4, 1923

By Andrew S. McCraeath

The treatment which a steel receives, and the uses to which it may be applied, are frequently determined by the percentage of carbon which it contains; and especially is this the case in the different steel works in this country. The part which this element plays in the composition of steel is such an important one that a process for its accurate determination becomes an absolute necessity.

By Thomas M. Brown

The method usually employed in accurate determinations of sulphur in pig-iron and steel is to treat a weighed sample of borings in a flask with muriatic acid, and to pass the gaseous products through an alkaline solution of lead or silver, which precipitates all the solphur of the sulphuretted hydrogen in the form of sulphide of lead or silver. The sulphide thus formed is subsequently oxidized by aqua regia, bromine, or other oxidizing agent, and the sulphuric acid formed precipitated in the usual way by chloride of barium. I have substituted for the alkaline metallic solution, a solution of permanganate of potash in the strength of one gramme of permanganate to 200 cubic centimetres of water, and find that it gives results quite as accurate as those obtained by using an ammoniacal solution of silver. By the employment of the permanganate it will be readily seen that there is considerable saving of time and work. In order to test the accuracy of the method, six samples of pig-iron borings were weighed out (about six grammes each) and treated identically

By Ralph Arnold

PERHAPS the most striking feature in the three newly discovered fields in the Los Angeles basin is the enormous thickness of oil sand. The total thickness is not yet known in any of the fields, since no well has as yet been drilled deep enough to pass through it. In the Signal Hill area a maximum of 1500 ft. or more of productive sand has been penetrated. In the other fields the interbedding of considerable shale members renders the total sand thickness somewhat less, but in all cases the depth of sand strata is enormous when compared with other California fields. For instance, in the Coalinga field the total thickness of sand on the average has been less than 100 ft., while in the Midway and Sunset fields not more than 250 ft. of actual productive sand has been encountered in any one place. This condition has so upset all previous ideas regard-ing the possible future production that but few of the engineers who have had to deal with the situation feel

Jan 5, 1923

The Institute published a collective index of- Volumes I to XXXV inclusive, which has been very extensively purchased and used by the members of the Institute. It enables one to look, up any subject in the first thirty-five volumes and is useful to those who have the Transactions, as well as to those who have not, because it tells what subjects have been treated and enables one to look these matters up in his own library and then afterward either to procure the individual papers from the Institute at the price of $1 each, or to procure Volumes, or to consult the Trans-actions at a nearby library, if such a one is available. It now seems desirable to publish another collective index, and the Editorial Department, upon the authority of the Board of Directors, has prepared an index of Volumes XXXVI to LV inclusive. This will be sold in the Institute's standard half morocco binding at a price of $5 and in paper covers at a price of $4. It wilt be ready in a few weeks. Those who already have the first index and purchase the second one, and those who purchase both, will have a complete index of the Transactions from Volumes I to LV inclusive. The Institute will be glad to receive advance orders for this index to insure prompt delivery upon publication.

Jan 8, 1917

By R. B. Brinsmade

The following is an attempt to form a formula by which a mine can be quickly evaluated, aft,er all pertinent physical data have been collected from observations on the ground by a competent mining engineer. Assumptions. Let Q = price to be paid for the mining property. M = cost of developing the mining property to yield y tons of ore daily. P = cost of suitable plant to treat y tons of ore daily, p = value of said plant when the mine has been exhausted. C = total fixed capital investment. W = working capital investment. Then let C + W = total capital investment. y = required yield of ore daily in tons. Y = yield of ore yearly in tons, d = number of producing days per year, u = average operating profit per ton of ore. R = rate of interest to be earned on total investment of (C + W). r = rate of interest to be earned on sinking fund annuity. v = tons of positive ore available in mine. x = tons of probable ore available in mine, z = tons of possible ore available in mine, m = fractional factor to change probable to positive ore. n = fractional factor to change possible to positive ore. Q = tons of total ore available in mine. t = time in years to exhaust mine at rate Y.

Jan 1, 1909

By Henry M. Howe

Henry M. Howe, Bedford Hills, N. Y. (communication to the Secretary.)*—Mr. Johnson's explanation, that the rounding of the graphite masses in oxygen-bearing cast iron is due to their being in part reprecipitated after re-solution in forming carbonic oxide temporarily with.that oxygen, is certainly most attractive and suggestive. It remains to be shown whether this rounding occurs also when the solidification is too rapid to permit this process to go on. J. E. Johnson might easily test this by casting a single ladleful of his oxygenated iron in masses of varying size. If this present hypothesis is true, then the rounding ought to increase progressively with the size of the casting, and with the distance from the outside, that is to say with the time available for re-solution and reprecipitation. I question whether a like benefit is to be expected even on this hypothesis, from the oxygenation of steel. The spheroidizing of graphite does good because graphite itself is so weak. But the constituent which can be spheroidized in steel is its cementite, which is a source of strength. Lamellar pearlite, in which this cementite in effect forms long den-drites, is far stronger than divorced pearlite, in which these dendrites have been broken up into spheroids. Even the surfaces of contact between ferrite and cementite are probably sources of strength because of the amorphous iron which probably fills them.

Jan 1, 1917

By Pradeep K. Rohatgi, Clyde M. Adams

Structures produced upon solidification of the eu-tectic composition (33 wt pct Cu) aluminum copper alloy have been examined as a function of freezing rate dfs /d? , the rate of change of fraction solid (fs) with time (8). Slow (dfs/d? = 0.0016 sec-1), intermediate (dfs/d? = 0.02 sec-1) and rapid (dfs/d? = 0.4 to 7.30 sec-1) freezing rates were used. The lamellar Al-Cual2 eutectic is arranged in the form of rod-shaped colonies at rapid freezing rates. The colonies are aligned parallel to the direction of heat flow, whereas the lamellae within the colonies are aligned at various angles, as high as 90 deg, to the direction of heat flow. The colony spacing (C) is proportional to the square root of inverse freezihg rate. The relationship is C = 15.5(dfs/d?)-1/2 where C is in µ and 8 is in sec. The ratio of colony spacing to lamellar spacing is greater than 20.0 and increases with a decrease in the freezing rate. A duplex dendritic structure is produced at intermediate freezing rates. A fine lamellar eutectic is arranged within the dendrites (exhibiting side branches at an angle close to 60 deg from the main stem) and a coarse irregular eutectic appears in the interdendritic regions. The duplex eutectic structure is also produced at slow freezing rates. However, at slow freezing rates there is a Platelat of CuAl2, along the center of the main stem of each dendrite and the other lamellae are arranged perpendicular to the central platelet. THE eutectic between CuA12 and a! aluminum has been reported to freeze in a lamellar form by several workers.'-3 chadwick4 has measured the interlamel-lar spacing as a function of growth rate. Kraft and Albright2 have reported on irregularities in the lamellar structures, and have proposed growth models which account for the formation of faults during solidification. In certain instances the lamellar eutectic has been found to exist in colonies. The colony formation315 has been attributed to the breakdown of a planar liquid-solid interface due to rejection of impurities. The aim of the present work is to study the structures produced from the eutectic aluminum-copper alloy under relatively fast solidification rates, such as encountered in casting and welding operations. The solid-liquid interface presumably remains planar under conditions of slow unidirectional freezing which produce lamellae aligned parallel to the direction of heat flow. The local growth velocities are the same over the entire interface and are equal to the rate of growth of the all-solid region. The spacing between the eutectic lamellae is inversely proportional to the square root of the growth rate of the all-solid region. Under the freezing conditions used in the present study, the solid-liquid interface is cellular or dendritic and the local growth velocities are different in the different regions of the interface. The relationship between the growth rate of the all solid region and the local growth velocities varies with the location and the shape of the interface. The growth rate of the all-solid region is, therefore, an inadequate parameter to describe the eutectic micro-structures which depend upon the local growth velocities. For this reason the structures have been examined as a function of freezing rate, dfs/d?, where fs is the fraction solidified at time 0. The freezing rate was varied by a factor of 4000. The relationship between the freezing rate, dfs/d?, and the growth velocit of the all solid region depends upon the specimen geometry and the shape of the interface. EXPERIMENTAL PROCEDURES The A1-33 pct Cu alloy used throughout this study was made in an induction furnace, using electrolytic copper and aluminum of commercial purity (99.7 pct), the primary impurities being silicon (0.12 pct), iron (0.14 pct), and zinc (0.02 pct). Three ranges of freezing rates were investigated: 1) A spectrum of rapid freezing rates (ranging from 0.40 to 7.30 sec-1) was obtained in arc deposits made on 2-in. thick cast plates of the eutectic alloy. The arc was operated at constant power and was made to travel at constant velocity on the surface of the plate that was in contact with the chill surface during solidification. The pool of liquid metal formed under the moving tungsten arc solidified rapidly by heat extraction through the unmelted plate. Conditions of unidirectional heat flow were achieved near the fusion zone interface, especially in the center of the arc deposits. The great advantage of the arc technique is that rapid cooling and freezing rates can be varied in a qualitative way. The correlation between the arc parameters and the solidification rate is given by the following relationship:6-8

Jan 1, 1970

By Charles Catlett

An examination of the census reports' for 1880, which contain a large number of complete analyses of typical American iron-ores, indicates that the existence of barium sulphate in intimate association with iron-ore is rather unusual. Of 94 analyses reported there, but four show any barium sulphate, and the maximum content amounts to 3.04 per cent. The note of the occurrence of considerable quantities of barite in connection with certain iron-ores found in the Pinar del Rio Province of Cuba may be of interest. These deposits are found near the little village of Francisco, about 25 miles west of the city of Pinar del Rio on the Western Railroad of Havana. The principal ridges are anticlines, and consist of very thick deposits of sandy shales and slates containing a large number of little veins of white quartz, which, by the gradual disintegration of the mass of the material, is left covering the surface. This quartz occasionally shows sulphide, but is generally barren of any such indication. At times lenticular masses of a more or less pure limestone mere observed in these slates. The shales, which are of light color, are occasionally talcose. The formation would tentatively be classed as the Lower Cambrian, arid the heavy ridges of comparatively horizontal limestone found in the anticlinal valleys as the Upper Cambrian. Along the crest of these slaty ridges deposits of iron-ore are found which are apparently in place, and were probably formed by replacement of masses of limestone similar to those noted elsewhere. The ready disintegration of the slates, arid the

Jan 1, 1908

By V. Pasupathi, R. E. Hummel, J. W. Koger

Specimens of P1 brass were plastically deformed at room temperature to various degrees of deformation and subsequently cooled in order to transform them to low-temperature martensite. Deformation shifts Ms. A, , and the temperature of minimum resistivity to lower temperatures, and also decreases the temperature coefficient of electrical resistivity. These properties change rapidly up to about 15 pct reduction but vary very little with higher deformation. The possible relationships between martensite formed by deformation and the M, temperature of low-temperature martensite are discussed. Evidence is given that deformation martensite delays the formation of low-temperature martensite. BETA' brass undergoes at least two different types of martensitic transformations. One of these transformations (B1- B2) was first observed by Kaminski and ~urdjumov' and occurs when 81 brass with a zinc content between 38 and 42 wt pct (quenched from the single-phase region) is cooled below room temperature. Jollev and Hull' determined the structure of 0" from X-ray and electron-diffraction data as ortho-rhombic. Kunze came to the conclusion that the super-lattice cell of 0" is one-sided face-centered triclinic (pseudomonoclinic). The second martensitic transformation (B1-A1) occurs when the specimens are deformed at or somewhat above room temperature. This type of martensite will be called deformation martensite. Horn-bogen, Segmuller, and Wassermann4 determined the structure of deformation martensite to be bct. (An intermediate phase, az, occurs before the final phase appears.) At deformations higher than 70 pct, a, transforms into a.4 A critical temperature Md exists above which no transformation occurs during deformation and is estimated to be around 400°C in P1 brass.5 This martensite has elastic properties.6 When the sample is stressed, martensitic plates appear; when the stress is released, the plates disappear. The present paper studies the effect of deformation martensite on the formation of low-temperature martensite. The experiments involved samples of 8, brass which were plastically deformed by various amounts and were subsequently cooled below the transformation temperature. EXPERIMENTAL PROCEDURE The 13 brass investigated was made from 99.999 pct pure copper and 99.9999 pct pure zinc and contained 38.8 wt pct Zn. The specimens, consisting of foils 0.1 mm in thickness, were heat-treated at 8'70°C for 15 min in an argon atmosphere and then quenched into ice water. They were then deformed by cold rolling and subsequently cooled at a rate of 1°C per min. The martensitic transformation that occurred during cooling was followed by electrical resistivity measurements. The resistance measurement technique and its accuracy have been described in a previous paper. Because the transformation 81 —-8" occurs below room temperature, the samples were placed in a cryo-stat which contained isopentane as a cooling medium. The isopentane was cooled by liquid nitrogen pumped under pressure through a 15-ft coil of copper tubing which was immersed in the isopentane. The nitrogen flow was regulated by a temperature controller using two thermistors in the cooling medium. The cryogenic liquid could be heated with an immersion heater. The useful temperature range with this device was from +25° to approximately -155~C. EXPERIMENTAL RESULTS Resistivity Measurements. The following abbreviations are used in this paper to label the characteristic temperatures during the martensitic transformation. M, is the starting point of the martensitic transformation and is defined as that temperature where the resistivity vs temperature curve on cooling first deviates from a straight line. Mf is the temperature at which the martensitic transformation is completed. On reheating, the transformation from martensite to the parent phase starts at a temperature A, and ceases at a temperature Af. Fig. 1 presents five different resistivity vs temperature curves corresponding to the transformation of brass from Dl to 8" after different degrees of reduction in thickness. The following observations can be made from these curves. 1) With increasing degree of deformation the Ms temperature is shifted to lower temperatures. This shift ranges up to 35°C compared to the undeformed state. This is also indicated in Fig. 2, where AM, (the shift of Ms, compared to the undeformed state) is plotted vs the degree of deformation. AM, increases rapidly until a reduction of about 15 pct is reached. With higher deformations, no additional increase in AM, was found. 2) With increasing degree of deformation the temperature of minimum resistivity (M) is also shifted to lower temperatures. The shift, attains a maximum of about 61°C compared to the undeformed state. In Fig. 3, AM is plotted as a function of deformation. It can be seen that, as in 1 above, AM increases rapidly and no further shift of M occurs for deformations greater than 15 pct. 3) The temperature coefficient of resistivity, is given by the slopes (dp/dT) of the linear portions of

Jan 1, 1969

By S. Skowronski, K. W. McComas

Page Purpose of investigation.....................'. 354 Details of experiments........................ 357 Experiment Series No. 1, melting copper containing chlorine under carbon dioxide............................... 358 Experiment Series No. 2, melting hydro-electric cathode copper drillings under air................................ 362 Experiment Series No. 3, melting hydro-electric cathode copper drillings under furnace gases............................ 363 Summary.............................. 364 Purpose of Investigation Since cuprous chloride melts at 418' C., boils at 954' C. to 1032' C.,' and is known to be volatile at a much lower temperature, the presence of chlorine in any form in or on copper to be melted has always been looked upon by copper refiners as a possible source of serious copper loss. Although this fact has been known for some time, the copper literature contains little or no information regarding it and the field seems never to have been properly investigated from a metallurgical standpoint. According to Greenawalt,2 cupric chloride, CuCl2, when ignited gives cuprous chloride; therefore cuprous chloride is always formed when copper enters into reaction with chlorine at a high temperature. Cuprous chloride melts somewhat below a dull red heat, and does not volatilize in closed vessels, even if strongly heated, but if heated in the air it goes off as a white vapor, Hofman3 gives the melting point of cuprous chloride

Jan 1, 1919

Jan 1, 1916

By Allan J. Clark, W. J. Sharwood

When the cyanide process came into general use, late in the nineteenth century, chlorination was quickly supplanted, but amalgamation yielded place more slowly, being still the major process at many plants, where it is followed by cyanidation of the tailings. The research work of the Denny brothers in South Africa' was probably the most important contribution of its time to the metallurgy of gold. By grading analyses of mill products, they pointed to the necessity of fine grinding to accomplish maximum extraction by cyanide. The work here described is merely an extension of the Dennys' method. Developing the fine-grinding principle, the steps of "crushing in solution" and of "all-sliming" were logical sequels, though both had been attempted early in the history of the cyanide process. Crushing in solution introduced certain complications in amalgamation; when "all-sliming " was adopted it was observed that the omission of amalgamation did not materially affect the total recovery. Thus the field of the older process has become much restricted, being at present confined to ores which, yielding freely to amalgamation, either are too low in grade to show an economic advantage in "all-sliming," or present chemical or other difficulties making the use of cyanide solution unadvisable during the crushing and preparation of the ore. South African ores are typical of the former class; Homestake ores are of both classes, but even in these instances the amalgamation work is being curtailed and greater burdens thrown on the cyanide plants. It is obvious that the time required for the dissolution of gold depends on the size of its particles. In an effort to determine the critical size, the following laboratory method was evolved. A standard amalgamation test2 had already been established, which involves the agitation of about 100 gm. of ore with 20 gm. of pure mercury, the latter then being separated and its gold contents determined. This method was applied directly to certain mill products with interesting results, a few of which may be noted here. The column "Free Gold" gives the value per ton thus amalgamated, as against the " Total Gold " determined by fire assay.

Jan 1, 1923

By Allan J. Clark, W. J. Sharwood

When the cyanide process came into general use, late in the nineteenth century, chlorination was quickly supplanted, but amalgamation yielded place more slowly, being still the major process at many plants, where it is followed by cyanidation of the tailings. The research work of the Denny brothers in South Africa' was probably the most important contribution of its time to the metallurgy of gold. By grading analyses of mill products, they pointed to the necessity of fine grinding to accomplish maximum extraction by cyanide. The work here described is merely an extension of the Dennys' method. Developing the fine-grinding principle, the steps of "crushing in solution" and of "all-sliming" were logical sequels, though both had been attempted early in the history of the cyanide process. Crushing in solution introduced certain complications in amalgamation; when "all-sliming " was adopted it was observed that the omission of amalgamation did not materially affect the total recovery. Thus the field of the older process has become much restricted, being at present confined to ores which, yielding freely to amalgamation, either are too low in grade to show an economic advantage in "all-sliming," or present chemical or other difficulties making the use of cyanide solution unadvisable during the crushing and preparation of the ore. South African ores are typical of the former class; Homestake ores are of both classes, but even in these instances the amalgamation work is being curtailed and greater burdens thrown on the cyanide plants. It is obvious that the time required for the dissolution of gold depends on the size of its particles. In an effort to determine the critical size, the following laboratory method was evolved. A standard amalgamation test2 had already been established, which involves the agitation of about 100 gm. of ore with 20 gm. of pure mercury, the latter then being separated and its gold contents determined. This method was applied directly to certain mill products with interesting results, a few of which may be noted here. The column "Free Gold" gives the value per ton thus amalgamated, as against the " Total Gold " determined by fire assay.

Jan 1, 1923

By Thomas M. Drown

The use of bromine as an oxidizing agent, particularly for sul phur, has become very general in analysis, replacing the stronger oxidizing acids. The object of this paper is to describe briefly the experience which we have gained with this reagent in the laboratory of Lafayette College in the oxidation of metallic sulphides. Most of the simple sulphides, as blende, pyrite, etc., when exposed to the combined action of an alkaline hydrate and bromine, and finally to hydrochloric acid, are completely and promptly dissolved. The procedure is as follows: The very finely pulverized mineral is first treated, in a beaker, with a solution of sodium hydrate of a spe cific gravity of 1.25, and heated ; bromine is then cautiously added to supersaturation, and finally hydrochloric acid to acid reaction. If any of the sulphide is not taken up, the same operation may be re peated. It is necessary, however, that the mineral be very finely pulverized. Instead of using the pure bromine, a saturated solu tion of bromine in potassium bromide may be used with equally good effect. The process is advantageously simplified by making a saturated solution of bromine in the concentrated alkali. This is done by pouring bromine into a solution of sodium hydrate, of the above given specific gravity, until no more is taken up, and then adding a little of the sodium hydrate solution until the liquid does not give off free bromine. The procedure with this solution is as follows: The pulverized mineral is moistened with, say, 10 cc. of the solution, and heated, then hydrochloric acid added to just acid reaction. Two more additions of the alkaline solution, in amounts of 20 cc. each, are added at intervals of about ten minutes, each addition being followed by hydrochloric acid. The total amount of the alkaline solution (containing the bromine) used is, therefore, 50 cc., and the amount of hydrochloric acid should not exceed that necessary to make the solu tion acid after each addition of the alkali. The mixture should be kept hot. After the final addition of acid, the contents of the beaker is taken to dryness and heated in an air-bath to 110° to 115°C., to render silica insoluble. The dry mass is then taken up by hydro' chloric acid and water and, after filtration, the sulphuric acid is pre

Jan 1, 1880

By H. F. Moore

We have studied the simple case of repeated stress, without considering impact, which might bring in other factors. This investigation has shown that steel under repeated applications of stress, reversed from positive to negative, will not fail below some fairly clearly defined limiting stress that, so far we can see, does not bear any definite relation to the ordinary elastic limit, being as large as the elastic limit in some cases and about one-half the elastic limit in others. According to one theory, fatigue is the result of changes in crystalline structure by repeated stress. I do not know of any evidence in favor of this theory. The crystals are broken under repeated stress. According to Bauschinger, under repeated stress some inherent property of the material changes its elastic limit; possibly some property of the amorphous cement between the crystals. A third theory is that all fatigue of metals is the result of the spread of damage from little localized overstresses. While I do not feel justified in accepting the last theory rather than the second, I have yet to run across a case of failure of steel or other metal, either in the laboratory or in service, that could not be explained by the gradual spread of damage from some nucleus. We have found, for example, that it is possible to subject a homogeneous steel, like Armco iron or a 0.90 per cent. carbon steel, that has been thoroughly annealed, to one hundred million reversals of stress as high as the elastic limit of the steel with no sign of failure. On the other hand, a complex structured steel, like a chrome-nickel steel that has been hardened with very little drawing, will fail at a stress about 58 per cent. of its elastic limit. Between these two we get a variety of results. In the steel work of any building, there are undoubtedly many thousands of places where structural damage was done—where riveted members were bent into place cold and where the rivets were fitted with drift pins, etc. Locally the steel in the building was stressed beyond its yield point in many places. These little localized overstresses do no damage at all; the building is entirely safe. But if this building were subjected eight or ten times a day to a mild earthquake, these little localized overstresses might be nuclei from which damage would spread

Jan 1, 1922

By R. Grierson, L. J. Bonis

The high-temperature Strength oF TD nickel has been observed to be dependent upon the previons thermal and mechanical history of the material. Variations in both the level and the anisotropy of strength have been observed. 01 this paper- these variations are correlated with the storing of annealing resistant elastic strain energy in the matrix of the TD nickel. An x-vay line -broadening tecknique is used to measure the maLrTis elastie strain. THE inclusion of a finely dispersed second phase into a ductile matrix has long been recognized as an extremely effective method of strengthening the matrix both at high and at low homologous temperatures. It has been found, however, that the factors which determine the high-temperature strength are not the same as those which are important at low temperatures. Below 0.5 Tm the size and distribution of the second phase particles are of prime importance in determining the strength,')' while above this temperature the strength is mainly dependent upon the previous thermal and mechanical history of the alloy,3-7 This paper is primarily concerned with explaining the response of the high-temperature mechanical strength of one of these alloys (DuPont's TD nickel) to various thermo-mechanical treatments. It will be shown that this response is not associated with the occurrence of any form of dislocation substructure within the matrix of the alloy. It has been found, however, that a correlation does exist between the elastic strain level in the matrix and the previous thermomechanical history of the alloy and that the observed changes in elastic strain level parallel the measured changes in high-temperature strength. It therefore must be concluded that variations in high-temperature strength are a direct result of the variations in elastic strain level. MATERIAL TD nickel contains approximately 2 vol pct of Tho2 in an unalloyed nickel matrix. It is formed, as a powder, by a chemical technique and this powder is compacted to form ingots which are then extruded to give 21/2-in.-diam rod. Rod of smaller diameter is prepared from the as-extruded rod by swaging. In the studies reported in this paper, 1/2-in.-diam rod was used. This rod received an anneal of 1 hr at 1100°C prior to being used in any of these studies. EXPERIMENTAL TECHNIQUES Two methods were used to examine the structure of the nickel matrix of the TD nickel. These were: 1) transmission electron microscopy; 2) the analysis of the position and profile of X-ray diffraction lines obtained using the nickel matrix as the diffracting media. To prepare thin foils for electron-microscopical examination, slices of TD nickel approximately 0.050 in. thick were cut from the as-received 1/2-in.-diam rod. These were then chemically polished down to 0.045 in., rolled to 0.009 in., given a predetermined heat treatment, and thinned, using a modified Bollman technique, to provide the foils for observation. All observations were carried out at 100 kv, using a Hitachi HU-11 electron microscope. Specimens of the undeformed rod were prepared by grinding down the 0.050-in.-thick slices to approximately 0.015 in. and then thinning chemically and electrolytically to give the thin foils. The X-ray specimens were prepared by rolling 0.375-in.-thick rectangular blocks down to 0.075 in. The surfaces of the rolled material were ground flat, chemically polished to remove the layer disturbed by the grinding, and given a predetermined anneal in an inert atmosphere. They were then ground lightly to check their flatness and given a final chemical polish prior to being examined. The X-ray diffraction line profiles were measured using an automated Picker biplane diffractometer. A special specimen holder was built to allow a more accurate and reproducible positioning of the specimen. The line profiles were determined by carrying out intensity measurements at intervals of either 1/30 deg or 1/60 deg over a range of 3 deg on either side of the nickel peaks of interest. A piece of pure nickel which had been recrystallized to give a large grain size was used as a standard to give the X-ray line profile generated by a strain-free matrix. The analysis of the X-ray diffraction line profiles is a modification of that due initially to Warren and Aver-bach8and has been described elsewhere.3 This analysis gives a measurement of two parameters associated with the structure of the nickel matrix. These parameters are: 1) the size of the coherently diffracting domains within the nickel matrix; 2) the magnitude of the elastic strains in these domains. Both of these parameters are first determined in terms of a Fourier series. These series are obtained from other Fourier series which describe the measured profile of the X-ray diffraction lines. Thus, for both the coherently diffracting domain size and the elastic strain level, it is possible to plot Ft (the Fourier coefficient) against t (the term in the Fourier series), where t can be expressed in terms of a distance L and the Fourier coefficient Ft(S) (associated with elastic strain level) can be expressed in terms of the root mean square strain (e2)1/2. Thus a plot of (F 2)1/2 vs L can be obtained. Plots of this type are shown graphically in Figs. 6 and 8. Interpretation

Jan 1, 1968