Search Documents

By R. A. Beall

Consumable-electrode arc melting is now accepted throughout the industry as the best method for producing ingots of zirconium, titanium, molybdenum, and their alloys. In addition, the technique is widely used in laboratories for fusing samples of such metals as hafnium, chromium, tantalum, columbium, and thorium. The production of consumable electrodes from these metals presents some rather difficult problems, the accepted industrial solution being the use of heavy powder-metallurgy-type presses. This paper summarizes information on fabrication of consumable electrodes by this and alternative means, such as sintering, nippling, and welding lightly pressed compacts of scrap metal. A possible saving of considerable capital investment is shown in the case of sintered compacts. The electrical circuit components of a pilot sintering unit are analyzed. INTRODUCTION The consumable-electrode arc-melting process has been accepted by most of the industry as the best method at present for producing high-quality pure or alloy in-got from sponge titanium or zirconium. This technique is not particularly new, having been patented by Von Bolton (l)3/ in 1909 for melting tantalum. However, it has been applied to industrial-scale operation only in the last few years. Among the important contributions to this technique are the work of Kroll (2) and Parke and Ham (3) and the work reported by the Office of Naval Research (4). The Bureau of Mines-has added considerably to the knowledge of this process (5-9).

Jan 1, 1956

By R. W. Huber

The successful development of a titanium prototype of the 81-mm. mortar base plate for the Army Ordnance Corps is outlined in this report. Information is presented dealing with forming, forging, and machining, welding and assembly techniques, and design changes relative to this prototype. INTRODUCTION The work of the Federal Bureau of Mines in making ductile titanium available2/ has resulted in the establishment of a new industry. Owing to its strategic importance and the combination of low density and high strength, titanium has received considerable attention as a structural metal. Titanium's favorable strength-to-weight ratio is of particular importance to the Army Ordnance for equipment that is transported by airplane or by foot soldiers.

Jan 1, 1956

By C. S. Allbright

This report gives the results of analyzing three groups of crude shale oils by the Bureau of Mines procedure:4/ (1) Oils produced by standard Fischer assay determinations on oil shales from Brazil (Paraiba Valley) and the United States (Colorado); (2) oils produced from Brazilian shale by different retorting methods; and (3) oils from high-temperature retorting of Colorado oil shale in the Entrained Solids retort. It is the second in a series presenting data obtained by analyzing crude shale oils from various sources. The series furnishes information on the general characteristics and compositions of a wide variety of shale oils. Use of a standard analytical method on all samples facilitates comparison of different oils. The 18 oil samples analyzed in this project comprised 3 from assays of Brazilian and Colorado oil shales in the Fischer retort, 9 obtained by processing Brazilian shale in various other units, and 6 from entrained solids retorting of Colorado shale at 1,000° to 1,500° F. The crude oils from Brazilian shale contained about half as much nitrogen as the Colorado oils. Properties of the Fischer assay oils from Colorado shales agreed with some data that relate grade of the oil shale with properties of the crude oil from the Fischer assay. Comparison of results from Fischer assays of oils from the foreign and domestic shales shows that the oil from Brazilian shale contains more low-boiling material and less residuum than either of the two from Colorado shale. This fact is reflected in lower specific gravity, viscosity, and carbon-residue values for the Brazilian oil. Retorting Brazilian shale in the Entrained Solids unit at 1,120° F. produced an oil whose boiling range was generally lower than the boiling ranges of oils obtained by processing in three other retorts at conventional temperatures. The quality of crude oils from high-temperature retorting of Colorado shale in the Entrained Solids process varies with retorting temperature. As the temperature is raised within the range 1,000° to 1,500° F., the amount of the naphtha fraction in the crude oil increases to about 35 percent and the aromaticity to 98 percent.

Jan 1, 1956

By P. R. Sperry

Aluminum alloy 3S was examined to determine the relationship between the applicable phase diagram and the microstructures produced under conditions tending toward non-equilibrium as well as equilibrium. The only phases present in the alloy were aluminum, (Mn,Fe)A16, aAI(Mn,Fe)Si, and silicon. It was found that the alloy behaved essentially as though it belonged to the Al-Mn-Si system. The effects of various solidification rates and of various homogenization treatments were studied. Particular attention was given to a nonuniform precipitate distribution which reflected the solute distribution in the cast aluminum solid solution. Some possible explanations for the solute distribution based on characteristics of the Al-Mn-Si or AI-Mn systems were discussed. ALUMINUM alloy 3s (aluminum plus 1.25 pct Mn) is one of the oldest and the most widely used of the wrought aluminum alloys. In spite of this fact, there are some aspects of the metallography of 3s which have not been revealed or which have not been brought to the attention of the metallurgist working with the alloy. The purpose of this investigation was to demonstrate in general how some of the fundamentals of equilibrium phase diagrams may be applied to the study of an alloy and to show specifically the origin of certain metal-lographic features of aluminum alloy 3s. It is hoped that this information can serve as a basis for solving specific problems relating microstructure to such things as mechanical properties, recrystallization, grain growth, and surface finish. Literature Survey Considering that alloy 3s contains only one alloying addition, manganese, it seems reasonable that it would have characteristics pertaining to the A1-Mn system. However, those characteristics might well be altered by the impurities in the commercial alloy, especially iron and silicon. Therefore, not only the simple binary but also more complex systems had to be reviewed. One characteristic of the A1-Mn system worthy of mention is its sluggishness, which leads to conflicting solubility data1,'2 and makes it relatively easy to supersaturate the solid solution and shift the eutectic composition during rapid solidification.3'4 Another characteristic is the strong influence which small amounts of impurities, especially iron, exert in lowering the solid solubility of manganese. Undissolved manganese is ordinarily present in an intermetallic phase, MnAl,, having an orthorhombic crystal structure. A metastable precipitating phase designated as "G" has been reported but small amounts of iron and silicon suppress this phase entirely." Raynor has established that MnA1, can dissolve a considerable amount of iron by a substitution of iron for manganese atoms up to 50 atomic pct.'" Consequently, in the Al-Mn-Fe liquidus diagram, the eutectic valley separating the primary aluminum and (Mn,Fe)Al, fields is fairly close to a constant Mn + Fe content." This is an important consideration in regulating the composition of 3s and also other aluminum alloys with high manganese additions."

Jan 1, 1956

By J. D. Sudbury, J. E. Landers, D. A. Shock

The external corrosion of casing is one of the most important problems facing the present day production man. A 1953 NACE report' estimated the annual cost of casing corrosion at $2,200,000 in 22 fields studied. The fields represented only 10 per cent of the wells in the United States. It was significant that 77 per cent of the failures reported were due to external corrosion. A variety of means for combatting the casing corrosion problem have been discussed in papers such as the NACE survey' mentioned previously. No attempt to revicw these will be made in this paper. Thc scope of this paper has been limited to a discussion of the following major items: (I) an instrument for studying external electrolytic corrosion; (2) use of this instrument to determine the quantity of protective current required to prevent corrosion of casing; and (3) problem of accelerated external corrosion of the oil string at the base of the surface string. ELECTROCHEMICAL MECHANISM OF CORROSION It IS gcncrally belleved that one major cause of external corrosion is the existence of electrolytic cells operating between various formation waters. A theoretical discussion of the role of earth potentials in casing corrosion has been presented by L. de Witte and F. J. Radd.2 A brief picture of the electrolytic corrosion action between two differcnt formations (A and B) is presented in Fig. I. This picture is a review to many but is given to insure clarity. In the anode area, oxidation takes place as iron ions go into solution in formation A as a product of corrosion. In the cathode area. reduction takes place and hydrogen atoms are formed at the boundary between the pipe and formation B. The flow of electrons. as indicated. is into the pipe at the anode or corroding area and out of the pipe into the formation at the cathode. In order to conform with regulations of this journal, the flow of a conventional current (I! is also indicated in this sketch. All subsequent references will be to this so-called conventional current flow and will be indicated by the symbol (I). As this action takes place the layer of hydrogen developed on the cathode offers a resistance to the flow of current in the cell. It is said (hat the cathode has been polarized. This polarizing film can be rcmoved by addition of a so-called dcpolarizing agent which reacts with and removes this hydrogen film. Such an agent must be present in ordcr for this corrosion reaction to go at a rate sufficient to cause a severe corrosion problem. The two common depolarizing agents are: (I) oxy-sen. which readily reacts with hydro gen to form water, and (2) certain bacteria which use atomic hydrogen as part of their life process. It is not difficult to explain the presence of these agents. Oxygen may be present in some very shallow formations. Sulfate reducing bacteria are found to exist in nearly any ground where mud pits might be dug. THE CASING POTENTIAl-PROFILE Instrumentation A sketch of the equipment* uscd in determining casing potential profiles is shown in Fig. 2. The tool is run in the hole using a hoist truck with a three-conductor cable. This tool must be run with tubing and rods out of the hole and should be run with the flow line disconnected. By proper choice of electrode size it can be run in any size casing. The electrodes must be run in an open hole or a hole filled with oil. Measurements cannot be made while immersed in water. The tungsten carbide-tipped knives serve as the electrical robes and arc spaced 25 ft apart. The potential difference along a 25-ft section of casing is measured with a potentinmeter to an accuracy of about 5 mv. Current flowing in the pipe can then

Jan 1, 1956

By O. C. Blade

This report on the properties of burner-fuel oils produced during 1956 was issued under a cooperative agreement between the American Petroleum Institute and the Bureau of Mines, United States Department of the Interior, at the request of the Oil-Heat Institute of America and the petroleum industry. This survey is the second for this type of fuel, the first being made in 1955. 2/ The surveys are conducted to provide information on the characteristics of burner-fuel oils now manufactured for sale. They are similar in pattern to the diesel-fuel surveys, conducted since 1950, 3/ and are not intended to conflict with but rather to supplement them. The importance of fuel oil has resulted in the need for more information by the petroleum industry, manufacturers of heating appliances, and consumers regarding the types and qualities of the fuels currently being marketed. Samples of burner-fuel oil typical of their manufacture during the early part of 1956 were analyzed by the refiners in accordance with instructions from the subcommittee on fuel surveys of the Automotive Research Committee of the American Petroleum Institute, Results of the analyses were transmitted to the Bureau of Mines where the data were studied and compiled as shown in the tables of this report.

Jan 1, 1956

By J. R. Low, M. B. Reynolds, L. O. Sullivan

The effect of neutron bombardment upon the stability of type 347 austenitic stainless steel has been investigated by a magnetic technique. The relation of the ferrite content of a stainless steel to its magnetic properties is given, and an apparatus suitable for the measurement of the ferromagnetic saturation induction of small specimens is described. Results of measurements on irradiated specimens are tabulated. Exposure to a neutron flux was found to cause a slight increase in the ferrite content of type 347 stainless steel, the change increasing with increasing length of exposure and with increasing initial ferrite content. The similarity of the effect of irradiation to the effect of annealing is pointed out. Possible effect of irradiation upon density of austenitic stainless steel is discussed. COMMERCIAL austenitic stainless steels are alloys of iron, chromium, and nickel, plus small quantities of other elements. Although these alloys are normally used in the austenitic condition, this state is thermodynamically metastable at ordinary temperatures and transformation to a more stable state takes place under favorable conditions. In the austenitic state, these stainless steels have the face-centered-cubic crystal structure characteristic of y iron, but the stable state at room temperature is a mixture of austenite and body-centered-cubic ferrite. The transformation from the pure austenitic condition may be brought about by cold working the alloy at a temperature below that at which the aus- tenite becomes thermodynamically unstable (about 400°C), the completeness of transformation increasing with increasing severity of cold work and decreasing temperature. The behavior of the austenitic stainless steels under ordinary conditions of use is rather well known. However, use of these alloys in a nuclear reactor introduces a new variable: the effect of neutron bombardment upon the transformation from the austenitic to the ferritic state. It was with this in mind that a study of the radiation stability of austenitic type 347 stainless steel was undertaken. Magnetic Technique for Ferrite Determination Commercial austenitic stainless steels such as type 347 undergo little transformation under normal conditions of fabrication and use. In view of this fact, it seemed likely that neutron irradiation would change the ferrite content of the alloy but little. The method chosen for measurement of the effect of neutron irradiation was thus limited to one which would be quite sensitive to small changes in the ferrite content of the alloy. Of the properties of the stainless steel which can be measured, the magnetic characteristics are most sensitive to the quantity of ferrite present.

Jan 1, 1956

By O. C. Blade

This report on the properties of aviation gasolines and aviation jet fuels produced in the United States during 1955 was made under a co-operative agreement between the American Petroleum Institute and the Bureau of Mines of the United States Department of the Interior. Analytical data are presented for 116 samples of aviation gasoline and for 38 samples of aviation jet fuel. The analyses were made on samples typical of the manufacturers' 1955 production in their laboratories and the results submitted to the Bureau of Mines for compilation. The products of 20 manufacturers of aviation gasolines and of 16 producers of aviation jet fuels are represented.

Jan 1, 1956

By P. Farrar, H. Margolin

The Ti-Pb diagram was investigated in the region 0 to 58 pct Pb and from 500°C to liquidus temperatures. Three reactions were encountered: I—ß?a+Ti Pb at 725 10°C; 2—ß+L?Ti4Pb at 1305+ 10°C; and 3—the possible eutectic L-+Ti,Pb and y between 1200" and 1300°C. LEAD-RICH alloys have been investigated by Nowotny and Pesl,' who used sintered compacts and studied the region from 37.5 to 100 pct Pb by X-ray diffraction analysis. The only phase found in addition to titanium and lead was the hexagonal compound Ti Pb. Alloy systems of lead with metals of the transition group, such as iron, chromium, tungsten, cobalt, nickel, or manganese, generally show little liquid or solid solubility.' Craighead et al.,3 however, indicated that lead is soluble in a and ß titanium to at least 2.1 pct. They also found that approximately 50 pct of the lead added was lost during the arc-melting of Ti-Pb alloys. In the present investigation, are-melting also was used to prepare Ti-Pb alloys and similarly large lead losses were encountered. Experimental Procedure Alloy Preparation: Considerable difficulty was encountered in the melting of the Ti-Pb alloys and a number of experiments were performed before the method described was developed. Alternate layers of lead and titanium were wrapped with titanium sheet and compacted. This "sandwich" was annealed at 300" to 350 °C and was melted according to the procedure described by Cadoff and Nielsen.' Using a low current, 150 amp, and an argon atmosphere, four to eight 10 to 20 sec melts were made on each alloy, with the button being turned over between each melt to insure homogeneity. In the high lead range, the preliminary sintering was found to be of doubtful value and was eliminated. In the region above the nominal composition of 70 wt pct Pb, the alloys prepared in this manner always consolidated into two phases. The outside appeared to be composed entirely of lead and the inside was a Ti-Pb alloy. In order to determine whether this phenomenon was caused by a miscibility gap, master alloys with a nominal composition of 40 wt pct Pb were machined and mixed with various percentages of lead sheet. This mixture was compacted and melted in the same manner as the other alloys. Although these alloys were not homogeneous, they did not show the layering that was observed

Jan 1, 1956

By Robert U. King, John W. Vanderwilt

THE Climax molybdenite deposit in Lake County 100 miles southwest of Denver is located in the central part of the mineral belt extending northeasterly across the state. Principal geographic features and geology are shown on Fig. 1. The first period of molybdenite mining, which began in 1918, ended in April 1919 because of limited demand and a price drop to about 72¢ per lb. During this time the ore came from the Leal level and surface outcrops at a higher elevation. Rate of mining was 250 tpd and several million tons of ore averaging 0.7 pct molybdenite were developed. Since April 1924, when the second period* began, Climax Molybdenum Co. has been the only operating company. Production in 1924 was 400 tpd and finding ore was a continual problem. When the White tunnel was extended, however, further ore was encountered. The orebody was thought to be tabular until 1926, when B. S. Butler recognized the relation of the developed ore on the Leal and White levels to a central area of fine-grained hydrother-mal quartz, and by 1929 diamond drilling had blocked out indicated ore reserves in excess of 100 million tons. In 1946, on the basis of information obtained from 25 miles of mine workings and a completed exploratory program involving over 200,000 ft of diamond drilling, the present authors reviewed and brought up to date the geology of the orebody. More recently Sears," employing microscopic techniques, made a study of hydrothermal alteration and mineralization, and Howell and Schassberger'" restudied available geologic data. Production (1953) of molybdenite ore has been expanded to over 25,000 tpd and total production from 1918 through 1953 has been: Tungsten, tin, and pyrite are byproducts and monazite also was produced from 1949 through 1951, after which it was not saved. A maximum of 15 to 20 tons of monazite was produced. Geology of the Area Pre-Cambrian crystalline rocks constitute most of the Mosquito Range for several miles to the north, east, and south of the Climax molybdenite deposit, see Fig. 1. To the west the crystalline rocks are in fault contact with shales and sandstones of Pennsyl-vanian age. Both crystalline rocks and sediments are intruded by dikes and sills of Tertiary age. Numerous faults with small displacements are to be found in the crystalline rocks east of the Mosquito fault and in the sedimentary beds to the west. Pre-Cambrian Rocks: The pre-Cambrian rocks consist of schist and gneiss, identified with the Idaho Springs formation, and granite with minor pegmatite correlated with the Silver Plume granite of the Silver Plume area. The Idaho Springs formation is a general term applied to pre-Cambrian schist and gneiss found over a large part of the Colorado Front Range. At Climax this formation consists largely of biotite-schist and quartz-biotite gneiss with minor quantities of plagioclase and orthoclase, although in places appreciable quantities of feldspar and quartz are present in the more gneissic varieties. Locally, especially along the contact with granite, recrystal-lization of the schist has produced coarser texture and a more pronounced than average gneissic appearance. The gneiss and schist have been mapped as a single unit by Butler and Vanderwilt (1933)" and by Singewald (1951).12 Schist predominates at the higher elevations of the Mosquito Range and in the area to the north and east of Climax. The regional trend of schistosity is northeast with varying dips to the east. Silver Plume granite and associated pegmatite intrudes the Idaho Springs formation. Silver Plume granite in many places and in the Climax district in particular has an irregular form, and many large and small inclusions of schist and gneiss occur within the granite. Granite predominates at the surface in the immediate vicinity of the area of hydrothermal alteration and extends for several miles to the northeast and southeast. As more schist is present at lower levels of the mine than in the upper levels, the suggestion is that the granite is sill-like in form,

Jan 1, 1956

By Jim Douglas, H. H. Rachford, D. W. Peaceman

The problem of unsteady-state gas flow through porous media has been solved numerically only for the case of linear or radially symmetric reservoirs. A recently introduced numerical method for solving the unsteady-state heat flow equation in two dimensions is applied to the calculation of the depletion of a square region containing a perfect gas. Solutions are presented in graphical form for various values of dimensionless parameters. The solutions are compared with published .solutions for radial reservoirs. I NTR ODUCTION The problem of unsteady-state flow of gas through porous media gives rise to a second-order non-linear partial differential equation for which no analytical solution has been found. Numerical approximations to solutions of the gas flow problem have been obtained by the stepwise solution of an associated difference equation1,2. However, the methods so far developed have required that the reservoir be either linear or radially symmetric. This restriction in shape has been necessary so that only two independent variables be considered, namely, one distance variable and time. In order to deal with reservoirs having more realistic shapes, it is necessary to develop numerical procedures for the solution of the gas flow problem involving two distance variables. A numerical procedure, denoted as the alternating-direction implicit method, for the solution of the heat-flow problem in two dimensions has recently been introduced" By the use of this procedure, approximate solutions have been obtained for heat-flow problems in a square8, and in regions having various non-rectangular boundariesa. Because of the similarity between the equation for heat conduction in solids and the equation for gas flow in porous media, it is reasonable to expect that the alternating-direction implicit method should also be useful for solving the gas flow problem in various two-dimensional regions. Solutions have been calculated for the simplest two-dimensional region, a square reservoir with a single well in the center. While reservoirs of such simple geometry seldom, if ever, exist, the solution of this problem is of some practical importance because it is also the solution of another problem, that of determining the depletion history about an individual well in an infinite uniform reservoir containing wells spaced throughout on a square lattice and producing equally from each well. Finally, it is of interest to compare solutions for a square reservoir with those for a circular reservoir and to determine the effect of the shape of the boundary for that particular case. METHOD OF CALCULATION Basic Differential Equation By combining the equation of continuity, the perfect gas law,

Jan 1, 1956

By J. T. Williams

The equilibria in the V-Zr alloy system were investigated by solidus temperature determinations, thermal analysis, dilatometry, electrical resistance measurements, microscopic examination, and X-ray diffraction analysis. There is a eutectic reaction at 1230°C between a compound, V2Zr, and a solid solution containing 10 pct V in ß zirconium. V2Zr decomposes at 1300°C into liquid and a solid solution containing about 10 pct Zr in vanadium. The eutectic composition is probably about 30 pct V. A eutectoid reaction between V2 Zr and a zirconium takes place at 777°C at a very high rate. The eutectoid composition is 5 wt pct V. The limit of solubility of zirconium in vanadium was estimated to be 5 pct at 600°C. No attempt was made to determine the liquidus for the system. THE recent availability of large quantities of high purity zirconium has stimulated the study of zirconium binary systems. The equilibrium diagram for the V-Zr system has received little attention, however. Wallbauml appears to have made the first report concerning the equilibria in these alloys. He reported the existence of a compound, V2Zr, having the MgZn2 ((214) type of structure with a, = 5.277 kX and c° = 8.647 kX. Anderson, Hayes, Roberson, and Kroll2 made a survey of some potentially useful zirconium binary alloys and found that zirconium probably dissolves a small amount of vanadium. They reported the probable existence of a compound between the two elements and suggested that the zirconium-rich solid solution undergoes a eutectic reaction with this compound. Pfeil," in a critical review of the existing information, estimated that the solubility of vanadium in zirconium is less than 4.7 pct and probably less than 1.8 pct. Rostoker and Yamamoto' proposed a partial diagram for the V-Zr system in a survey paper on vanadium binary alloys. Their diagram indicates the compound, V,Zr, a eutectic reaction at 1360°C, a peritectic reaction at 1740°C, and a limit of solubility of zirconium in vanadium of about 3 pct. They obtained no information on the equilibria in the zirconium-rich alloys. In view of the potential utility of the V-Zr alloys and the incomplete knowledge concerning the equilibria in the system, an attempt was made to establish the constitutional diagram. Preparation of the Alloys Raw Materials: The vanadium for making up these alloys came from the Electro Metallurgical Corp. Zirconium came from two sources. In the beginning of the investigation, sponge zirconium from the Bureau of Mines was used in making some of the alloys. Later, iodide metal made at the Westinghouse Atomic Power Development Laboratories became available. This material was used in the preparation of all the dilatometric and resistance specimens and about two-thirds of the solidus temperature specimens. A typical manufacturer's analysis of the vanadium is shown in Table I. No other analysis of the vanadium was made. The metal contained a dispersed second phase and did not have a sharp melting point. Typical results of spectrographic analysis of the Westinghouse zirconium are shown in Table 11. These data indicate a very high purity. The Bureau of Mines sponge metal was probably less pure but had good ductility. Melting: All of the alloys used in the investigation were made by melting pieces of vanadium and zirconium together in a dc electric arc furnace similar to those of Geach and Summers-Smith, craighead, Simmons, and Eastwood," and others. Melting was done in an atmosphere of helium scavenged of residual air by the preliminary melting of a separate charge of zirconium. Each ingot was turned over and melted at least three more times before removal from the furnace to aid in the attainment of homogeneity. Alloys prepared for use in the investigation are listed with the results of solidus determinations in Table III with the exception of the following compositions upon which no solidus determinations were made: 0.29, 0.54, 4.57, and 5.55 pct V. Analysis: The weight of each ingot made from iodide zirconium was within 0.1 g of the total weight of the initial charge, about 90 g. Since each component of each charge was weighed to the nearest 20 mg for amounts less than 10 g and to the nearest 0.1 g otherwise, the gross composition of an ingot could be calculated accurately. Chemical analysis for the vanadium content of several alloys agreed

Jan 1, 1956

The presence of undetonated explosives in a rock face after firing constitutes a hazard which can result in a fatal or serious accident if undetected before drilling commences.Most accidents caused by drilling into explosives are the result of failure to examine the working face properly and lack of care in subsequent drilling operations; it is not always realized that explosive may be left in the butts of holes or may be driven into cracks or crevices in the rock.Obviously the best means of preventing accidents of this nature is to adopt methods of drilling, charging and firing which will reduce the hazard to a minimum.There are three ways in which undetonated explosives may be left in the rock face, namely:1. Misfires.2. Cut-off shots.3. Incomplete detonation or failure of the charge to propagate throughout.MisfiresNo attempt will be made in this paper to deal fully with the question of the prevention of misfires, as apart from the fact that most of the preventive methods are well known, it is believed that if the miner receives his explosives and means of initiation in good order, and proper care is taken in their use, the failure of a charge to fire will be a rare occurrence. The provision of central fuse capping stations on mines has gone a long way towards the elimination of misfires caused by the mishandling of safety fuse anddetonators.

Jan 1, 1956

By J. D. Edwards, C. S. Taylor, A. S. Russell

Solubilities and densities are reported for alumina hydrates in NaOH solutions under the conditions of the Bayer process employed to purify alumina for aluminum production. The equilibrium constants for reactions to form A102- accurately correlate the effects of NaOH concentration on the solubilities; the temperature coefficients of the equilibria lead to heats of solution of 7.34, 4.76, and 5.24 kcal for the a trihydrate, a monohydrate, and ß trihydrate, respectively. Moderate calcination does not change the solubility of the a trihydrate but increases that of the a monohydrate. At solution temperatures above 100°C, the trihydrates transform rapidly to a monohydrate. Hydro-thermally produced a monohydrate is the stable phase above 20°C. CORNERSTONE of the aluminum industry, the Bayer process for alumina production is based on the difference in solubility of hydrated alumina in NaOH solutions between 170" and 40°C. Solubilities and densities in this system were determined thirty years ago by M. Tosterudl under the direction of J. D. Edwards and C. S. Taylor. The solubility data, which still appear more concordant than those in the literature, are employed to sort out the complex equilibria in this system. The nomenclature for the alumina hydrates is that presented in The Aluminum Industry' and more recently summarized in Alumina Properties.3 a trihydrate is the purified phase analogous to gibbsite, a monohydrate is similarly akin to boehmite, and ß trihydrate is sometimes known as bayerite. Literature Goudriaan4 reviewed the early literature on alumina in NaOH solutions and presented data on the solubility at 30°C of several forms. The gel precipitated from aluminum sulphate or chloride with ammonia and dried at 130" to 140°C had the highest solubility but was unstable, its solubility being cut to one-tenth on standing in NaOH. The solubility of the gel was decreased one-third on calcination at 300" to 400°C, while that of the gel transformed in NaOH at room temperature to a crystalline trihydrate was unchanged on calcination. The preparation produced by slow hydrolysis of sodium aluminate solution with CO, in the air gave solubilities in rough agreement with later values for a trihydrate. The solubility of this form was increased slightly by the calcination. Fricke and Jucaitis5 extended the work to 30" and 60°C with a trihydrate. They also gave solubilities for ß trihydrate (bayerite b), although the residue belonging to the left branch of the solubility curve corresponded to a trihydrate. The residues at high NaOH concentrations were mono and trisodium aluminates, the latter being 3Na2O . AL2O3 • 6H2O. Solubilities of a trihydrate at 95°C and of a monohydrate at 150" and 200 °C come from the work of Magarchak.6 a trihydrate transformed to a monohydrate above 95°C. A few measurements on the solubility at 25°C of an alumina trihydrate prepared by slow hydrolysis of NaAIO, solutions were presented by Sprauer and pearce.? Their analyses showed the monosodium aluminate to have the composition Na2O.Al2O3-2.5H2O.

Jan 1, 1956

Established as a Division December 15, 1948 Clayton G Ball, Chairman Louis C Raymond, Vice-Chairman Sheldon P Wimpfen, Vice-Chairman Henry T Mudd, Vice-Chairman A H Lindley, Jr, Secretary-Treasurer Division of Foreign Activities U S Bureau of Mines Washington, D C

Jan 1, 1956

By C. G. Albert

The clay particles of 2 microns or less required for modern paper coating are predominantly flat plates, lying smoothly on the sheet and producing a high gloss. Operating speeds of today's coating machines necessitate a clay composition of 60 and sometimes 70 pct solids as against the 35 to 40 pct required in the past. Since clays in suspension may solidify in flow, only those of intrinsically low viscosity can be used as high coating solids. THE literature of paper technology contains a number of articles having reference to developments in the field of coating and filler clays for use in paper manufacture. Much of this information has not been included in mining publications and has therefore not been readily available to all in the mineral industry. Recent developments in this field, including spray drying of clays, are presented here. U. S. Bureau of Mines figures for 1952 indicate that the paper industry consumes more than 50 pct of all kaolin produced and sold in the U. S. As most of the kaolin used by the industry comes from Georgia producers, the fraction of their output destined for paper use is thus appreciably higher than 50 pct. Small wonder that the kaolin industry, especially in Georgia, is highly sensitive to the quality requirements of paper mills and must respond promptly to technological developments in paper manufacturing. The paper industry itself is not the ultimate consumer. For the greater portion of the clay the end product is the printed page, and the demands of printing and publishing have sparked some of the technological advances in paper making which have, in turn, brought about methods employed in the kaolin industry. As compared with the product of 20 or 25 years ago, one of the most striking characteristics of the graphic arts today is the mass production of quality printing of fine pictorial work, much of it in full color. During this time periodicals with printing standards close to those of yesterday's slick-paper publications that were printed on a slow schedule and for a limited circulation have grown to the point where they go out to many millions of readers, often at weekly intervals. The complexity of technological improvements brought about by this increased circulation is probably not appreciated even by technical people, unless they have had reasonably close contact with the industry. The advance has come about through developments not only in the art of printing, but also in the field of paper making and even at the level of clay mining and processing. The smoothness required for faithful reproduction of the kind of printed matter under consideration is attained with a clay-coated paper. Since the distribution expense of the publication will depend to a great extent on its weight, the paper used must not be too heavy. This means a lower basis weight than was normal for conventional clay-coated papers some 25 years ago. And for this mass production market it becomes necessary to provide a paper having these and all the other required characteristics at a very moderate price—not the premium price conventional clay-coated papers formerly demanded. This challenge has been met by a new method of producing coated paper. In the past, application of clay coating to paper was a conversion operation, performed separately from the making of the base sheet. The newer development is called machine coating. Here application of the coating is an integral step in a continuous process by which wood pulp, clay, and other ingredients are manufactured into a sheet of coated paper. Many more problems are involved in this procedural change than are apparent at a casual glance. The coating operation, for example, must function at much higher linear speed than could be obtained with coating mechanisms previously employed. The application machinery developed to meet this requirement necessitated changes in composition of the coating color.* This created new requirements, summarized below, for the clay employed as coating pigment. In addition to smoothness, a relatively glossy printing surface is needed, and to a large measure it is the function of the coating clay to make possible the development of both these surface characteristics. Traditionally, pigments such as satin-white, prepared by reacting lime with paper-makers' alum, were used to assist in producing a high finish. However, economic considerations and others preclude large-scale use of such material in the new processes. In the 1930's Maloney' discovered that a certain particle size fraction of kaolin, consisting

Jan 1, 1956

By E. R. Palowitch

This report is the result of a series of coal-cleaning tests using a dense-medium cone-type washer. Detailed results are given for 2 tests using a magnetite medium and 4 tests using a pulverized-refuse medium. Approximately 120 float-and-sink tests and over 500 separate chemical analyses were made in conjunction with these tests. In these tests higher recovery efficiencies and sharper separations were obtained when using a magnetite medium, especially on coal sizes below one-half inch. When sizes above 1 inch at low specific gravities of separation are cleaned, the pulverized refuse medium compared favorably with the magnetite medium.

Jan 1, 1956

By R. H. Frazier, C. H. Lorig, F. W. Boulger

This investigation establishes the effect of ferrite grain size resulting from various heat treatments on the transition temperature of a semikilled steel plate. Different austenitizing temperatures and various cooling rates were used. The ductile-brittle transition temperatures were determined by the Navy tear test and the keyhole Charpy test. THE data presented in this paper deal with quality characteristics of ship-plate material which were investigated in a research project sponsored at Battelle by the Bureau of Ships, Dept. of the Navy. Specifically, the object of this investigation was to establish the effect of ferritic grain size (resulting from various heat treatments) on the so-called transition temperature of ship-plate steel. Transition temperature is not a fixed property of steel. It is derived from a series of static or dynamic tests made at various temperatures and is qualified by specifying the type of test employed as well as the testing criteria. Because in earlier investigations of ship-plate quality1,2 the so-called Navy tear test and standard notched-bar tests (keyhole Charpy) proved to be useful in interpreting instances of brittle behavior of ship plate in service, these tests were used in the investigation reported in this paper. By definition,' in the Navy tear tests the highest temperature at which one or more of four specimens breaks with a brittle fracture (that is, when less than 50 pct of the fracture area has a dull fibrous texture) is termed "transition" temperature. In the Charpy tests, the 12 ft-lb level of energy absorption was used as a criterion indicating the "transition" temperature, although other levels of energy absorption were also used for comparison. Earlier work" on ship-plate steels indicated that the temperature at which ship plate is finished has a very significant effect on its notched-bar properties. Plates rolled in the laboratory, where the finishing temperature can be carefully controlled, showed a 16°F decrease in tear test transition temperature when the finishing temperature was lowered 200°F (from X" to Y°F). The same plates showed a drop of 10°F in the keyhole Charpy transition temperature from the same decrease in finishing temperature. Commercially finished plates' exhibit a similar trend. When the ferrite grain size of the hot-rolled laboratory plates was determined, a close relationship was found between the ferrite grain size and the notched-bar transition temperature." " he indicated relationship between grain size and transition temperature was in agreement with the findings on low carbon steels of Hodge, Manning, and Reichhold' despite the differences in composition of the steels. The cooling rate after rolling varies from one steel plant to another. This variation changes the micro-structure" and appears very likely to affect the notched-bar properties of the steel plates. In the investigation summarized in the present paper, heat treatments simulating finishing practices in the hot rolling of ship plate were used in order to vary the ferritic grain size. It is believed that the indicated relationship between grain size and transition temperatures of the ship-plate material will prove useful in estimating the effect of rolling temperature and of cooling rates from rolling temperatures on the notched-bar properties of semikilled steel plate. Material The semikilled steel plate used in this investigation was a ¾ in. hot-rolled plate from an open hearth heat. Other plates from this heat have been used on many other studies performed for the Ship Structure Committee," "," and the heat has been identified as project steel "A". The chemical composition of the plate1 was 0.25 pct C, 0.49 pct Mn, 0.011 pct P, 0.045 pct S, 0.04 pct Si, and 0.004 pct N.

Jan 1, 1956

Jan 1, 1956

By P. Bardzil, J. Gurland

An experimental study of the variation of transverse-rupture strength with composition Anexperimentaland grain studysize has shown that the strength reaches a maximum for values of the mean free path between carbide particles of 0.3 to 0.6 microns. The fracture oforiginates in and proceeds through the carbide grains mainly. Impact strength and hardness also were recorded. MOST of the physical properties of sintered carbides vary linearly with composition. The transverse-rupture strength, however, shows a unique behavior. As the amount of binder metal is varied from 6 to 25 pct by weight, the strength at first increases; then, between 15 and 20 pct Co, it reaches a maximum of nearly 400,000 psi, and finally decreases with further additions of binder metal. This behavior of the transverse-rupture strength has been reported, among others, by Englel and Sandford and Trent.' The significance of these observations has not been discussed in the literature. That it may be of more than specific importance is indicated by the very similar variation of strength with composition encountered in other systems sintered in the presence of a liquid phase, such as Tic-Ni3 and Fe-Cu.' Experimental Details All compacts were prepared and sintered according to normal industrial practice. The average diameter of WC grains and the mean free path between grains were measured on metallographically prepared samples by a method of linear and planar analysis sing the relations where d is the average diameter of dispersed grains; Nl is the number of noncontiguous grains intersected on a metallographic plane by a line of unit length; N, is the number of noncontiguous grains per unit area; P is the mean free path between grains of dispersed phase; and f is the volume fraction of dispersed phase. Approximately 1000 grains were counted on each sample. For each composition d2 was plotted against P, the resulting straight lines serving as a check on the measurements. The distribution curves of the WC powders of different average diameters were homologous, and no attempt was made to influence the grain size by blending powders, adjusting the sintering conditions, or otherwise altering the particle size distribution. Densities were measured by differential weighings in air and water. The degree of densification did not vary consistently with either composition or grain size. The density is influenced by slight amounts of impurities, specifically by 0.1 to 0.2 pct Fe which enters the powders during ball milling. As an illus- -tration of the experimental variations, a number of measured densities are listed in Table I. They are expressed in percentage of theoretical density, as calculated from the published X-ray densities of WC and Co.' For the purpose of determining the transverse-rupture strength, rectangular test specimens (3/16x 3/8x3/4 in.) were broken by loading at the center of a 9/16 in. span. The average strength of five or more samples is reported for each composition and grain size. The compacts were ground on two parallel surfaces only. The load was applied at an average rate of 6,800 psi per sec. Since the elongation after fracture of the alloys is very small, it was assumed that the compacts deform elastically to failure and the fracture stress was calculated by the conventional beam formula. The data for one alloy are presented in Table II as an example of the results and scattering ranges encountered. The precision of the test, as measured by the average difference between duplicates, is of the order of 15,000 psi. The results are strictly comparable only to compacts prepared and tested in the manner described and of similar chemical composition and grain size characteristics. Unnotched Charpy specimens were used for impact testing. Each point represents the average of 3 to 20 samples, the larger number being used in an attempt to determine the influence of grain size. Considerable scatter was encountered, the range from lowest to highest value often amounting to 30 pct of the impact strength. The hardness is reported as a Ra reading, using a 60 kg load with diamond brale indenter. Compositions are given in weight percent.

Jan 1, 1956