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By George R. Eadie

As 1972 slipped through our grasp, coal industry adjustments to health and safety laws, environmental restrictions, rising costs and higher production targets left many mine operators groping for a new grip. The industry adopted a defensive attitude in 1972 as it faced the onslaught of inspectors. With rigid demands for improving safety and instituting environmental programs, the industry worked hard and watched production figures stagger upward while operating costs zoomed. In an effort to determine how to meet the goals that were established for fewer ignitions, fewer accidents, less respirable dust, lower noise levels, fewer law violations, better reclamation, less pollution, lower costs and higher production, industry representatives attended numerous technical meetings.

Jan 2, 1973

By J. C. Scully, G. Sanderson

The electrolytic formation of y hydride in thin foils of Ti-5Al-Z.5Sn alloy and four Ti-A1 binary alloys has been studied by electron microscopy and electron diffraction. Two orientation relationships have been found: THE adsorption of hydrogen by titanium alloys from aqueous solutions has been widely reported. This can occur, for example, in both alkaline' and acidic2 pickling baths, in chemical polishing374 and electro-polishing Solutions,3,4 during cathodic polarization5" and under certain corrosion conditions,7,8 Etching reagents may also produce visible precipitates, sometimes after an aging period.9 During an investigation into the stress corrosion susceptibility of a titanium alloys by thin foil electron microscopy many observations have been made of hydride precipitation which has been deliberately promoted by techniques that are described below. The characteristics of hydride precipitation are reported and the observed crystallographic orientation relationships are discussed with reference to distortion in the titanium lattice created by the presence of the hydride. EXPERIMENTAL TECHNIQUE One grade of commercial titanium and five alloys were examined. Their composition and hardness values are shown in Table I. All the materials were in the form of thin sheet, 0.05 to 0.065 cm thick, which had been annealed after cold rolling. Foils suitable for transmission electron microscopy were made in two ways: a) by chemical polishing; and b) by elec-tropolishing. The solution used for chemical polishing was a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. During this polishing specimens were manually moved up and down in the solution. The reaction was veFy rapid, specimens thinning to foil thickness (2000A) in 5 min. Since chemical polishing solutions tend not to cause hydride contamination if they are kept cool3 no attempt was made to prevent the solution from becoming hot during the thinning operation. Electropolishing was performed at -30° C with a mixture3 composed of 295 cu cm methyl alcohol, 175 cu cm n-butyl alcohol, and 30 cu cm perchloric acid with an applied voltage of 40 v after chemically thinning specimens to approximately 0.017 cm thickness in a cool solution of 44 pct HF, 40 vol H2O2, and water in the volumetric ratio 1:6:3. EXPERIMENTAL RESULTS 1) Ti-5A1-2.5Sn Alloy. The Ti-5A1-2.5Sn alloy was severely contaminated by hydrogen during the chemical polishing. Foils obtained in this way contained large amounts of the y hydride phase. A typical micrograph is shown in Fig. l. The laths were identified as the hydride phase by selected-area diffraction of a large number of foils examined in a tilting stage that could be turned through 40 deg. Using the lattice spac-ings of the alloy obtained by X-ray diffraction as a standard the a value of the hydride was determined fromo the electron diffraction patterns to be 4.38 to 4.40A. The accuracy of this figure is only about ±2 pct. Further evidence of the identification was obtained by vacuum annealing chemically polished foils of the alloy at 500°C. This resulted in the dissociation of the hydride with the production of dislocations and possibly vacancy loops as shown in Fig. 2. The hydride

Jan 1, 1968

By S. A. Braley

THE first commercial production of bituminous coal in the United States was in 1820, and formation of acid in the areas from which the coal was removed began at that time. Thus it is 130 years since the development of mine acid began. The coal operator has had to deal with the acid water produced in his mines, and his losses from corrosion of pumps and equipment have been tremendous. Other industries and the public have been forced to spend large amounts for their water requirements because of the acid discharge from the mines. There are many contradictions in the literature on this subject probably because of variations in the analytical procedures followed and differences in the methods of calculation and reporting. The opinions previously expressed may be summarized as follows: The production of mine acid has been looked upon as a simple chemical reaction wherein the oxygen of the air has reacted with pyrite to produce ferrous sulphate and free sulphuric acid. This reaction appears in many chemistry texts and generally has not been considered worthy of further study. Since the measurement of hydrogen ion concentration or activity was developed and expressed in terms of pH, indicator and instrumental methods for pH determination have become readily available, making it natural to think of it as a measure of acid content. Special purpose analytical methods applicable to potable waters, sewage effluents, and boiler waters, based in general upon the determination of what may be regarded as impurities, have been applied to more concentrated solutions constituting mine discharges, without reference to the fact that these specialized procedures had been developed to serve as operating guides for water-treatment plants. It has been assumed that the pounds of acid deliv- Table I. Showing pH and Titratable Acid of Varying Concentrations of Ferrous and Ferric Sulphates Ferric Ferrous ion Acldfty Ion Acidity (Fe+++) ppm CaCO3 We++) ppm CaCOa ppm PA equiv. PPm pH equiv. 11.200 1.80 30,000 11,200 3.98 20,000 5,600 2.01 15,000 5,600 4.15 10,000 2,800 2.21 7,500 2,800 4.41 5,000 1.120 2.48 3,000 1,400 4.68 2.500 560 2.60 1,500 140 5.00 250 280 2.65 750 28 5.00 50 112 2.81 300 56 3.07 150 28 3.38 75 ered by a mine was roughly a constant varying with the number of acres mined, and that the concentration of the acid in the drainage was inversely proportional to the volume of flow. Increased flow was thought to result in a dilution of the acid produced. When the Sanitary Water Board of the Commonwealth of Pennsylvania established a fellowship at Mellon Institute, the first approach to the problem was to review some of the chemical reactions involved and their relation to acid production. Since the sulphates of iron were among the principal constituents of coal-mine drainage, the first studies were based upon solutions of chemically pure ferrous and ferric sulphate. These are both neutral salts, that is, the iron and the sulphate are equivalent, but they produce acid reactions in water solution because as salts of strong acids with weak bases, they hydrolyze to form acid solutions. Solutions of each salt, of varying concentrations, were prepared and the pH, titrable acidity and iron and sulphate

Jan 1, 1952

By S. S. Shen, M. J. Pool, P. J. Spencer, J. R. Guadagno

VERY few thermodynamic data are available for rare-earth alloys, partly because of the difficulties of obtaining the metals in sufficiently pure form and also because of their comparative scarcity up to the present time. The rare earths form a very interesting series in the periodic table in view of the progressive filling of their 4f subvalence electron shell and would be expected to provide useful information with regard to alloying characteristics of transition elements. It has been found in recent calorimetric investigations that the heats of solution of a number of the rare-earth metals in liquid tin are highly exothermic.1-4 Exceptionally strong bonding between rare-earth and tin atoms is clearly indicated in the liquid solutions. Continued thermodynamic studies of the behavior of rare earths in solution could thus contribute a great deal to present theoretical knowledge of alloying behavior and would yield an insight into bonding of a strength hitherto unencountered in liquid alloys. The determination of the heats of solution of the pure components in liquid tin is an essential preliminary to calorimetric work of this nature. Heats of solution of praseodymium, neodymium, and samarium in liquid tin at 750" ' and the heats of mixing of Pr-Nd solid solutions' have already been determined in this laboratory. The present investigations with lanthanum continue the study of rare-earth elements. Details of the construction and operation of the liquid metal solution calorimeter used in this work have been published previously by Pool and Peluso and no further description will be given here. The lanthanum used in heat of solution determinations was supplied by Lunex who quoted the purity as 99.9 pct. Their detailed analysis of the material is given in Table I. Samples of 0.0003 to 0.0005 g-atom were used for each run and great care was taken to remove all surface oxide prior to weighing. The samples were stored at all other times in a beaker of oil to prevent their otherwise rapid oxidation. The compounds LaSn (Cudu, L1P type structure) and La&, (structure not classified) were prepared from the appropriate quantities of the two pure components by arc melting under a purified argon atmosphere and once again great precautions were taken to avoid any subsequent oxidation of the specimens. Although no structural examination of the compounds was made, the consistency of thermodynarnic measurements carried out on twenty or so individual samples of each indicates that the compounds were in fact homogeneous, single phase alloys. Samples of the compounds consisting of 0.0003 to 0.002 moles were used in the calorimetric measurements. A solvent bath consisting of approximately 80 g of 99.9 pct pure Sn was used for each series of runs and its heat capacity was determined at regular intervals throughout the experiments using pure tin or tungsten calibration samples. Measurements were made of the heat of solution of lanthanum in liquid tin at 725", 750C, and 775°K and at compositions up to 2.21, 4.76, and 5.25 at. pct La at the three temperatures respectively. In every case, the heat of solution of lanthanum remained constant at its limiting value, within experimental limits, up to the highest lanthanum concentration investigated. Since no change in was observed, it was concluded that the liquid/liquid + LaSn, phase boundary had not been

Jan 1, 1969

By D. R. Spink

In the preparation of zirconium and hafnium metals, there are many indications that impurity levels control the physical and chemical properties of the metal. The purpose of this work was to develop methods of producing pure raw materials that could be reduced to highly pure metals. Early work by the Carbomcndum Metals Co. and others indicated that certain fused salts were highly efficient in the removal of impurities from gaseous zirconium tetrachloride. We have developed workable fused salts along with a continuous and higly efficient scrubber design which can be used to produce very pure zirconium tetrachloride. Metal made from the purified tetrachloride has been shown to approach crystal bar metal in purity. Scrubber designs are discussed with recommended materials of construction. VARIOUS methods have been used to purify zirconium (and hafnium) tetrachloride. Most of these methods involve thermal degassing initially (the removal of more volatile compounds at temperatures below that where zirconium tetrachloride exhibits a significant vapor pressure) followed by a sublimation step (which conveniently leaves the nonvolatiles behind.) While these procedures effect definite purification, such processing is batchwise and does not result in optimum purification. Early work by The Carborundum Metals Co. and others indicated that fused salts were highly efficient in the removal of impurities from gaseous zirconium tetrachloride. The objective of this work was to develop a continuous fused-salt scrubbing process that would yield high-purity zirconium and hafnium tetrachlorides. The term "fused salt" refers to the molten state of ionic compounds and as used here, specifically refers to alkali metal and alkaline earth halides. Fused salts, because of their many valuable properties, are becoming increasingly im- portant industrially. These valuable properties of the fused salts are: 1) stability at elevated temperatures; 2)low vapor pressure; 3) low viscosity; 4) ability to dissolve many different materials; and 5) good elctctrical conductivity. All but the last property enhances the use of fused salts as scrubbing agents for zirconium and hafnium tetrachlorides. Fused-salt scrubbing may be defined for our purpose as the intimate contact between a gaseous compound and a molten salt with the purpose of removing impurities from the gaseous compound. In this case, the gaseous compound is zirconium tetrachloride which submlimes at 331°C. When this gas is contacted with a molten salt, impurities such as aluminum, iron, and titanium are removed and the resulting product is considered fused-salt scrubbed. Zirconium and hafnium are sold to a purity specification. Generally speaking, normal production without scrubbing is capable of meeting specifications. There are, however, several considerations That make the knowledge of methods of additional purification highly desirable. These are: 1) the control of product analysis; 2) the production of a pure product for special applications; 3) the salvaging of off-specification material; and 4) the use of raw materials with higher impurity levels than 1 he present raw materials. You will note that items 1 and 2 are somewhat complementary to each other and that item 4 assumes that The present process has impurity removal limitations. To better understand the part that fused-salt scrubbing of zirconium tetrachloride plays in the manufacture of zirconium, Fig. 1 contains an illustrated flow sheet of the industrial production of zirconium metal. In referring to Fig. 1, we can point out the specific benefits derived from our ability to purify zirconium tetrachloride. Purification of the crude (hafnium-containing) zirconium

Jan 1, 1962

By Robert Glass Cleland

THE DEATH of William E. Dodge occurred at a time when, all unwittingly, the company in which he had so long been the dominant factor was about to break with its old practices, its old traditions, its old interests, and transfer its major activities three fourths of the way across the continent and engage in an enterprise that differed almost as much from the original Phelps Dodge undertakings as the rough, arid mountains of the new region differed from the green hills and valleys of New England. To understand the effect of this transformation upon the fortunes of Phelps Dodge, one must change the setting of the present narrative from the familiar locale of the Atlantic seaboard to the land of "distance, silence, and solitude," that men called Arizona. In 1880 that Territory was one of the last frontiers of the Old West. To the Spaniards it had been a land of mystery and fable, the limit of the King's settlements, the far edge of the rim of Christendom. Through it Coronado; in a vain effort to find the fabulous Cities of Cibola, had led "the most brilliant company ever assembled in the Indies to go in search of new lands." Below its southern border, Father Kino, the "steel-thewed" Jesuit described by his

Jan 1, 1952

By C. E. Silverblatt, D. A. Dahlstrom

Previous bench-scale studies demonstrated that a substantial moisture reduction can be obtained by the application of steam to coal filter-cakes, particularly to those containing a limited amount of minus 200-mesh material. Consequently, U.S. Steel's Applied Research Laboratory conducted a study to determine the feasibility of steam filtration of 1/4 in. by 0 coal on a continuous pilot-scale installation in which an Eimco extractor is used. The test results showed that the moisture content of this coal could be reduced to 5.5% at a steam loading of about 175 lb of steam per ton of dry cake. In terms of steam consumption, this loading is calculated to be 1-1/2 lb of steam per lb of water removed. In some tests, only 1 lb of steam per lb of water removed was required. These levels of steam consumption are significantly less than the actual heat requirements of conventional thermal dryers. The satisfactory moisture reductions were obtained at filtration rates of 125 to 186 lb of dry solids per sq ft per hour. However, the proper design of commercial filters should improve the potential rates that can be attained. These results indicate that steam filtration has considerable economic potential for drying 1/4 in. by 0 coals and also has additional advantages over the conventional thermal drying of coal. The results of the previous bench-scale studies and those published by Burton' demonstrated that a substantial moisture-content reduction can be effected by the application of slightly superheated steam to coal filter-cakes, particularly to those containing a limited amount of minus 200-mesh material. Consequently, US Steel's Applied Research Laboratory conducted a study to determine the feasibility of steam filtration of 1/4 in. by 0 coal on a continuous basis. In the continuous process, the dewatering operation on the filter is conducted in stages. In the first, the bulk of the water in the feed slurry is removed by conventional mechanical dewatering on a portion of the filter before the steam is applied. In the second stage, steam is applied to the cake. The steam condenses and releases its latent heat, thereby reducing the viscosity of the remaining cake water; this reduced viscosity then facilitates further drainage and produces a cake of lower moisture content. Because of the availability of feed coal on a continuous basis and since steam was readily available from a low-pressure boiler, the Applied Research Laboratory selected for the test site a coal-preparation plant that cleans Pittsburgh Seam coal. A slurry of table and flotation coal in percentages as they occur normally was used as feed stock. Typical analyses of this slurry are shown in Table I. DESCRIPTION OF FILTER AND EXPERIMENTAL PROCEDURES An Eimco Extractor was selected for the evaluation of steam filtration in a continuous process. This unit was chosen because of its availability and its design features that permit relatively simple hood construction, instrumentation, and operation. A photograph of the Extractor is shown in Fig. 1. In the filter a cloth medium is used that travels horizontally and continuously with a grooved, rubber drainage belt. The total effective filter area was 12.5 sq ft. As the feed slurry flows by gravity from the feed box onto the medium,

Jan 1, 1964

By Glenn C. Waterman

Richard Strong (Oliver Iron Mining Div., U. S. Steel Corp.)—Mr. Waterman states (p. 59, Trans., January 1954): "Core-sludge combining factors have been calculaied for any combination of core-sludge recovery on the basis of several logical assumptions: 1—The sludge sample loses reliability geometrically as sludge recovery drops. 2—The sludge sample should not be used if the percentage of sludge return is less than the percentage of core recovered. 3—A core sample should receive a weighting at least equal to the percentage of core recovery." Assumptions 1 and 2 seem justified at Chuquicamata and most geologists would agree to the validity of assumption 3. However, contrary to the statement quoted above, the core sample does not in general receive a weighting at least equal to the percentage of core recovery when the Chuquicamata methgd is used. Furthermore, the basic Chuquicamata method is identical to the Longyear or relative volume core-sludge assay combining method. Finally, the Chuquicamata method does not, in its present form, reflect true geometric loss in sludge sample reliability according to the relationship L = AR (N-1) The basic equations representing the two steps of the Chuquicamata method can be combined algebraically as follows (using the symbology of the original article except as noted): Vol A + B Assay 2 = ASA = Assay 1 Vol A VolB Core Assay [I] Vol A CA.F + ASA (100 —F) Combined grade =[21 100 Pct where F and (100 — F) are the core and adjusted sludge assay factors from Fig. 3. Substituting Eqs. 1 and 2 and collecting terms Combined grade = Vol B Vol A + B CAF (100—-F) + Assay 1 (100-F) Vol A Vol A 100 pct Eq. 3 is a unified and general statement of the Chuquicamata method. The true core factor includes not only the factor F from Fig. 3 but also the quantity VolB ------------- (100 — F), which is implicit in the value of Vol A the adjusted sludge assay. This quantity is real and positive for all values of F and core recovery less than 100. Therefore the true core factor is always less than F except when F is equal to 100. If sludge recovery is 100 pct, Eq. 3 can be further simplified as follows: Let F = percentage of core recovered. Let Vol A = Vdh (100 Pct — Pct CR) where Vdh is the total volume of the sampled interval and let Vol B = (Vdh — Vc.) Pct CR where V, is the core volume in the sampled interval at 100 pct core recovery. Then combined grade = Vo V. CA Pct CR- + Assay 1, 100 Pct — Pct CR Vdh Vdh [4] 100 Pct Eq. 4 shows that when sludge recovery is 100 pct the laboratory sludge assay receives significant weight in the Chuquicamata method, even at 100 pct core recovery. The maximum weight assigned to the laboratory sludge assay depends on drillhole size, as follows: Eq. 4, with suitable changes in symbology, is identical to Royce's formula 8,' which is a statement of the Longyear or relative volume method of combining core and sludge assays. If Mr. Waterman's assumption 3 is of paramount concern to the geologist, the Royce method (for core recoveries of 60 pct and above) or a method employing the percentage of core recovered as a core weighting factor are the only recognized methods known to the writer which achieve the desired result. A modification of the latter method embodying Mr. Waterman's assumptions 1 and 2 would result from applying the factors from Fig. 3 directly to the laboratory core and sludge assays.

Jan 1, 1956

By R. A. Esmonde

This paper describes the building and testing of a prototype welded aluminum truck body to a new design concept. The results of these tests are given along with an outline of further developments in the design and field application of aluminum bodies. The results of field service history are recorded with special reference to types of mining operations, service performance, wear, maintenance and economics of operation. Mention is made of current U.S. usage and predictions given as to future development of aluminum bodies in the mining industry. The use of aluminum for off-highway truck bodies in hauling rock for the mining and construction industries is by no means the novelty that it may seem. In 1932 an aluminum unit proved very satisfactory in service on the Hoover Dam project but at that time the only high strength aluminum alloys available were not weldable and with the high cost of construction, a sound economic case for an aluminum body could not be made. After World War I1 great advances in aluminum welding techniques, using the inert gas shield, combined with the development of high strength alloys with good welded properties and welding characteristics changed the whole picture. Welded aluminum bodies were rapidly developed and by 1958 attention was again focused on the use of aluminum for off-highway truck bodies. EARLY DEVELOPMENT WORK In 1959 Alcan, the Aluminum Co. of Canada, embarked on an extensive development program to prove the durability and economics of aluminum truck bodies for the mining and construction industries. The first step was to design a prototype aluminum body which took particular advantage of the fact that the modulus of aluminum is only one third that of steel. This means that within the elastic range, aluminum moves three times as much as steel which makes it more flexible and capable of absorbing much greater impact shocks. A body was built and mounted on a 22-ton truck and taken to the Jeffery Mine of Canadian Johns Manville Company at Asbestos, P.Q., Canada. Very little information was available as to the order of stresses that were set up in off-highway truck bodies and so it was therefore decided to carry out a test program to find out this information.

Jan 1, 1969

By W. J. Parton

D. R. MITCHELL*—The Chairman mentioned that we have had many papers on cleaning of fine coal and treatment of wash water solids. There are, of course, two reasons for that. One is that we have legislation, particularly in the east. that is making us go into these things whether we want to or not. It just so happens at the present time that I have four plants that are going up under my general direction, three new and one rehabilitation job, and in all of them, we have these problems. Therefore, I was very happy to be able to listen to these papers, because some of the things that are in them are going to help me solve some of the problems that I am facing. Of course, the second reason why we are concerned about fine coal recovery is the fact that coal has become a luxury item in a good many places, particularly in the anthracite region, so that we cannot afford to have it go to waste like we did in former years. There is a third minor reason, and that is that we are finding how to handle and use the extremely fine sizes that we did not know how to use in former years. Now, I have a couple of questions that I would like to ask. First, what are the maximum solids that you could have in a pulp going to one of these launder screens? I realize that it would be for anthracite. Second, of course the life of these screen surfaces is not very long— with brass or bronze, I believe it is a week, and with stainless steel, a month. Would it be possible to use screen surfaces like the Bixby-Zimmer round rod for the small sizes and possibly increase the life? Have you experimented with that? Another point that I would like to bring out, both in Mr. Parton's paper and in some of the others, in studying cyclones and any settling apparatus where we use orifices, the life of the orifices is very short, and that is a problem that still has to be solved. The capacity of the cyclone seems to be small, and if you have a bat-

Jan 1, 1950

THE following employment items are made available to AIME members on a nonprofit basis by the Engineering Societies Personnel Service, Inc , operating in cooperation with the Four Founder Societies Local offices of the Personnel Service are at 8 W 40th St , New York 18, 100 Farnsworth Ave, Detroit, 57 Post St , San Francisco, 84 E Randolph St , Chicago 1 Applicants should address all mail to the proper key numbers in care of the New York office and include 6c in stomps for forwarding and returning application The applicant agrees, if placed in a position by means of the Service, to pay the placement fee listed by the Service AIME members may secure a weekly bulletin of positions available for $3 50 a quarter, $12 a year MEN AVAILABLE Executive Engineer, 37, married, 3 children Now Resident Manager nonmetallic underground mine and processing plant Management and operational experience in gold, copper, zinc, limestone and lime products manufacture Mine plant design and construction, underground mines and quarries Excellent references Currently employed but available reasonable notice Prefer U S M-687-426-E-5-San Francisco Metallurgical Engineer, 29, married, one child, B S Metallurgical Engineering Five years' practical experience in milling and laboratory research Available thirty days Prefer West or Southwest U S A M-689¬522-E-1-San Francisco Experienced Mining Engineer, university graduate, 40, married Twenty years' experience all phases metal mining, past 13 years as manager, excellent cost and safety record Available short notice Best references and complete professional record available upon request M-690

Jan 1, 1952

By David Reger

ONLY a few small pools of oil were found in West Virginia during 1924. The price of oil was so low that there was no incentive for active effort toward the discovery of new pools or the exploitation of reasonably certain productive areas. At present, several encouraging edge-pool developments are being held in reserve in the hope that a more favorable market is not far distant. In the old pools, wells are being carefully tended; there being little tendency toward abandonment. even in cases where production is temporarily unprofitable. In natural gas, however, the total value of which at the well mouth is now more than that of oil, the year has been busy and profitable. , The decline of old pools, together with the increasing demand, has caused the large operators who carry their gas to the consumer to make great efforts to preserve or increase the rate of production; while the small operators, who sell their product to the large companies at the well mouth, have been stimulated toward the same effort by more favorable prices. These conditions brought about the completion of a greater number .of gas wells in 1924 than in 1923. Few pools of gas have been discovered during the year, the principal production having been obtained in old areas and in the unusually large new territory that was revealed as potentially productive by the drilling of 1923. Some of these latter areas are still without pipelines but definite plans for getting most of this gas are now being executed.

Jan 3, 1925

By N. E. Grosvenor

Several methods have been proposed for determining the tensile strength of rock. These have been tried out over the past several years, but the results have been erratic and of doubtful value. The tensile strength of rock is its weakest property, and this property apparently enters into all failure phenomena, whether underground or on the slope of an open pit. Therefore, it is essential that detailed quantitative information is known about the tensile strength of rock if the design engineer is going to select the proper pit slope, pit orientation, or orientation of underground workings so as to give the most economical and safest mining condition. This quantitative information may be used to orient the pit in such a manner as to allow steep slopes along two sides. This information possibly may be used to orient the direction of either underground workings or open pits so as to decrease powder consumption and to increase blasting efficiency. Hence it is of prime importance that a method of determining accurately the tensile strength of rocks be developed. The U. S. Bureau of Mines states' that no standard methods have been proposed by the ASTM for testing the tensile strength of rock. The method described in the Bureau publication is said by them to be unsatisfactory. A similar test that has been used in our laboratory in place of the USBM test is shown in Figs. 1 and 2. h this test the core is placed in a set of grips that has been designed for one particular size core. The grips are designed to distribute the stress around the core if they are tightened correctly. A universal joint or a flexible cable may be used in conjunction with the apparatus to prevent bending or twisting of the specimen. The main difficulty encountered with the system shown is the failure of the specimen within the grips. The possible cause of the failure within the grips may be due to a stress concentration set up by the uneven tightening of the grips. This method can be used only for tests on cores, and even then has been found to be totally unsatisfactory because of the failure within the grips. The U. S. Bureau of Reclamation has been using a test similar to the sketch shown in Fig. 3. Sulfur is cast around each end of the specimen to form a bearing surface and then a ring grip is used to apply a tensile stress. The grips are in contact with the sulfur cast and do not touch the specimen. This method is unsatisfactory, apparently because a large number of the specimens appear to break within the sulfur cast. Professor Wuerker of the University of Illinois uses the test shown in Fig. 4.' Professor Wuerker states2 that this method has given definite and reproducible results with the weakest as well as with the strongest rocks. The test is a supplement in all cases where cores cannot be obtained. The principle and equipment are the same as for the test for tensile strength of hydraulic-cement mortar. Soft

Jan 1, 1961

By W. C. Knopf, G. Samsel

For several years International Minerals & Chem-ical Corp. has used a radiation method to assay potassium content of products from potash and feldspar beneficiation. The procedure is rapid, accurate, and inexpensive and is easily handled, if necessary, by nontechnical personnel. Data are presented to show the accuracies that may be expected if the technique is used for control of pilot plants or large-scale plants. Natural potassium is composed of three isotopes —K, K and K. Five other isotopes, artificially produced, have been detected. In natural potassium only the K isotope, with a half life of 1.4x10 years, is radioactive. Its modes of decay are beta and gamma rays, positrons, and x-rays. Only the more abundant beta rays, however, are important in radiation measurements using geiger tubes. Barnes and Salley' measured radiation of potassium salts in solution in 1943. Gaudin and Parnell2 first reported the use of solid salts arranged in a vessel surrounding the ß counter in 1948. Later, Scheel used the method to assay potassium content of various crude and finished potash salts. Experimental: Dip-type Geiger-Muller tubes (TGC-5) supplied by Tracerlab Co. were used in all radiation counting measurements. The tube was encompassed by a glass container about M in. larger in diameter than the tube. This container, which served as a sample holder, was closed at the bottom with a rubber stopper to facilitate removing the samples. Samples were not weighed, but about 40 g of sample were needed for each test. Electrical impulses from the tube were counted on either a Tracerlab scaler or a rate meter. To obviate the need for constant attendance, preset features were incorporated into the scalers, so that at a predetermined time or count the units were automatically deactivated. When rate meters were used, counting rates were read directly from instrument or from a recorder used in conjunction with the rate meter. Each tube was calibrated, according to the manufacturer's instructions, to determine the correct operating voltage to insure reproducible results. A linear calibration plot of percent K2O vs counting rate was also obtained for each tube by recording the counting rate plus background count of several standards of different K2O content chemically analyzed by the chloroplatinate method.' These standards were of approximately the same particle size distribution as samples to be assayed. Specific background count caused by cosmic rays and other surrounding radiation was checked periodically by counting a sample of pure NaCl. Fig. 1 is a representative calibration plot. Assays were determined directly from the standard plot or calculated by subtracting the background count from the counting rate, then multiplying by the slope of the line. Chemical assays of the test samples were made by the Sherril method," a flame photometric technique, or the chloroplatinate method. Data: The radiation assay method has been used for three years by International Minerals & Chemical Corp. in the laboratory and in pilot plants processing ores containing potassium. These dry concentration plants process sylvinite and langbeinite ores at Carlsbad, N. M., and feldspar ores at Top-sham, Maine. Sylvinite ore is predominantly a mixture of syl-vite (impure KCl) and halite (impure NaCl). Contaminants include sulfates, such as langbeinite (2MgSO - K2SO4), kieserite (MgSO H2O), poly-halite (MgSO4.K2SO, 2CaSO, . 2H2O), and slimes. Langbeinite ore is predominantly langbeinite and halite with small amounts of sylvite, sulfates other than langbeinite, and slimes. Several variables, in addition to correct calibration and standardization of tubes, were found to be important in obtaining reproducible results. Particle size distribution of standard samples should be

Jan 1, 1959

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

THERE has been considerable discussion among A metallurgists and others interested in the development of titanium alloys as to the nature of the fine line markings which appear in the microstruc-tures of unalloyed titanium and a titanium alloys. These markings have been variously called x phase, etching pits, and twins. Figs. 1 to 3 show typical examples of the line markings as they appear, respectively, in high purity iodide titanium, commercial purity titanium rod, and a high purity a alloy containing 0.2 pct N. The commercial purity titanium sample, shown in Fig. 2, contains both line markings and some spheroidal retained-ß phase. The ß phase seen in this micrograph should not be confused with the line marking, since it originates from the iron present as an impurity in the sponge metal. It will be noted that the line markings seem to have a definite orientation pattern with respect to the grains and in titanium noticeably resemble the precipitation occurring in artificially aged high purity Al-Cu alloys. This similarity led to the hypothesis that the line markings observed in titanium and a titanium alloys resulted from precipitation of some unknown phase. With the work of Hägg1 and McQuillan2 as background, there was little reason to suspect hydrogen of being responsible for the line markings. Hagg reported that up to 33 atomic pct H was soluble in a titanium, and McQuillan reported an a solubility of up to 8 atomic pct. Furthermore, McQuillan examined metallographically a 5.1 atomic pct H alloy quenched from 300°C and stated that the structure appeared to be a single-phase a solid solution. Line markings have been observed frequently and were first noted by Jaffee and Campbell3 in 1949. They did not observe them in vacuum-annealed titanium and a Ti-O and Ti-N alloys, but did observe them in Ti-H alloys containing 0.25, 0.5, and 1 atomic pct H. They stated that it was doubtful that the markings were a second phase based on hydrogen, because 1 atomic pct was far from the accepted solid solubility of hydrogen in titanium. Finlay, Resketo, and Vordahl,4 in 1950, concluded that the markings were a true second phase as a result of observations on their etching characteristics. Anderson5 Commenting on these markings in titanium was inclined to associate them with hydrogen, but was loath to call them titanium hydride, because of the reported high solubility of hydrogen. Work at Battelle Memorial Institute for the Navy Bureau of Aeronautics," done concurrently with the work described in this paper, provided information on the experiment converse to that described by Jaffee and Campbell in 1949. This work showed that the amount of line markings in unalloyed titanium could be decreased by vacuum annealing at elevated temperature. It was suggested that this was the result of removal of hydrogen; previously, the data of Jaffee and Campbell9 howed that the markings appeared when hydrogen was added. Recent work at Battelle for the Ordnance Corps, Department of the Army, which is described here, now establishes the identity of the markings as a titanium hydride phase. A sample of high-purity titanium rod 1/4 in. diam, 0.009±0.001 wt pct H (0.43 atomic pct), Fig. 1, was resistance heated in a 0.05 micron vacuum for 41/2 hr at 1500°C. During the early states of heating, the pressure increased to 150 microns, indicating that gases were being evolved. After cooling in vacuum, the iodide titanium rod was analyzed for hydrogen. Vacuum-fusion analysis showed 0.0006 ±0.0003 wt pct H (0.03 atomic pct) to be present.* Metallographic examination of the vacuum-annealed rod showed only a transformed ß structure. There was no evidence of fine line markings, Fig. 4. A section of this vacuum-annealed rod was cold rolled to 0.040 in. thick sheet and annealed for 1 hr

Jan 1, 1953

By Michel Elle, John Chipman

The equilibrium of gaseous H20-H2 mixtures with liquid iron-columbium alloys in the range 0.2 to 2.4 pct Cb shows that the activity coefficient of oxygen is strongly diminished by Cb. The oxide in equilibvium with the melt is identified as CbO2. The equi-librium constant at 1600 deg C is [%Cb][fo. % 0]2 = 2.9 x 10-4 where log fo= —0.14 [%Cb]. The deoxidizing power is comparable to that of vanadium, COLUMBIUM (niobium) is finding increasing use as an alloying element in steel. It forms several stable oxides and is removed from the steel bath by oxidizing slags. The specific oxide formed in steel-making is not known although Sazanov snd Shvarts-man,' in their study of its partition between slag and metal, have assumed this to be Cb2O5 It is the purpose of this study to determine its deoxidation equilibrium at 1600°c, the nature of the oxide formed and the interaction between columbium and oxygen in the melt. The investigation was based on the reaction H2 + O=H2O; Kl=ph2o/(pH2[%O]) [1] in which 0 signifies oxygen dissolved in the liquid Fe-Cb alloy. The method and equipment of recent studies2,3 were utilized. In brief, the molten alloy, contained in a small crucible, is held in a controlled mixture of steam, hydrogen, and argon until equilibrium is reached. It is then cooled quickly in a stream of helium and analyzed for columbium and oxygen, the latter by vacuum fusion.4 The solubility of the oxide in liquid iron is determined by visual observation of scum formation on the surface of the melt. Crucibles of MgO proved unsatisfactory because of partial reduction at the metal interface. Pure A12O3 crucibles were heavily blackened by the melt and could not be used at high concentrations of columbium. Silica crucibles were more satisfactory but these introduced some silicon into the melt thus necessitating an uncertain but small correction for its effect on the activities of the other solutes. In silica it was possible to observe the scum formation when the melt became saturated and there was no apparent reaction between scum and crucible. The procedure for saturated melts was as follows. The alloy charge composed of electrolytic iron and columbium grain was melted and held at constant temperature. The gas ratio H2O:H2 was progressively increased by raising the saturator temperature until a point was reached at which a bright film appeared on the surface and covered it completely. This film could be dissolved by raising the temperature of the melt and it reappeared when the temperature was lowered. Under a partial film covering, utilizing bare areas for temperature measurement, the melt was brought to equilibrium with the atmosphere by holding at temperature for about 1 hr as suggested by Dastur.5 INTERACTION IN THE MELT Several experiments were made without columbium to establish a base in silica crucibles. The results are shown in Table I. Except for one run, they agreed well with Floridis1 comparable results in other crucibles. The value of log K1 is taken from Table I as 0.58. This is slightly larger than Floridis' result, probably because of less elaborate safeguards against thermal diffusion. Results obtained in the Fe-Cb-0 series in which no scum formed are shown in Table 11. The equilibrium ratio Kl is defined as ph2o/(ph2[%O]). It is related to the equilibrium constant K1 as follows:

Jan 1, 1962

By D.E. Norquist, J. E. Moeller

The results of wear on marked balls, 4, 31/2, 3, and 2 in. diam are given. All balls were forged steel of practically the same chemical analysis and hardness. The results indicate that balls in a given mill for a given length of time will have equal diameter losses, regardless of size. IN order to determine the relative wear rates of several sizes of grinding balls, groups of 4, 31/2, 3, and 2 in. balls were marked individually and were charged, all at the same time, into each of two production mills grinding copper ore. The remainder, and vast majority, of the ball charge consisted of 2 in. diam, and smaller, white, cast iron balls. The original weight of each test ball was determined and recorded. Some of each group of test balls were recovered from the mills periodically, individually reidentified, and reweighed. The test balls were recovered during regular maintenance shutdowns, at approximately thirty-day intervals, so as to avoid disrupting operations. As soon as the weights had been recorded, each marked ball was recharged into the mill from which it had been taken. The test units were mechanically the same and theoretically received equal tonnages of feed. All of the test balls were of forged, alloy steel composition with only slight variations in chemistry that would not be expected to affect the physical properties. All were heat treated in the same manner to produce a high hardness, as equal as possible for all sizes and as uniform as possible from surface to center. Generally speaking, the hardness of the portion worn from the balls during the test ranged from 62 to 65 Rockwell C. The microstructure was, therefore, predominately martensitic. The method of marking the test balls consisted of forming a small, round hole, 3/16 or 1/4 in. diam, into the center of each test ball with a Thomas Metal Master disintegrator, which produces a hole in fully hardened steel without affecting the hardness of the surrounding metal. After the hole was formed, each test ball was individually weighed to the nearest gram and the weight was recorded. The balls were grouped as to size and each group assigned a code letter. The individual balls within the various groups were then assigned a number. A small copper disc was stenciled on one side with the group letter and on the other side with the individual ball number and dropped into the hole in the corresponding test ball. The hole was then plugged with a low-melting-point metal alloy, which could be melted out in boiling water. Half of the test balls in each group were charged into one mill and the other half into another mill, so that all test balls in each mill would be subject to, as nearly as possible, identical conditions for an equal length of time. Previous testing had indicated that the wear rates on balls of different sizes could not be accurately compared if weight loss, or percentage weight loss, were used as a basis for comparison. Fig. 1 is a graphic record of the average weight loss for each size group in mill No. 1, and it becomes readily apparent that the larger balls lose substantially more weight in a given length of time. Fig. 2 is a graphic record of the average percentage weight loss for each size group in mill No. 1, illustrating that the smaller balls definitely lose a greater percentage of their original weight in a given length of time. It was, therefore, decided to convert the actual weights of the test balls to diameter and follow the diameter losses periodically to see if the wear rates

Jan 1, 1951

By N. K. Chen, R. Maddin

Columbium single crystals were deformed in tension and compression. Reorientation by X-rays and stereographic projections of slip traces indicate that plane of slip may be considered as (110). The plastic behavior is shown to be quite similar to the deformation of molybdenum single crystals. STUDIES on the crystallography of the deformation process in body-centered cubic metals have been renewed recently with investigations of iron single crystals1-" and molybdenum single crystals.4 It is now apparent that too many exceptions to the rationalization based upon the ratio of absolute testing temperature to absolute melting point by Andrade5 exist to permit more serious discussion of this type of analysis. The considerations of resolved shear stress utilizing only planes of the type {ll0}, {112), and {123)³,6 permit analysis of the deformation only on the basis of those three types of planes. The suggestions made by Elam7 and by Greninger8 in which the slip process is envisioned as a composite slip on two nonparallel {110) planes can be illustrated schematically in Fig. 1. It may be seen that an unresolved trace on any plane containing a <111> direction may be accomplished by varying the number of atoms participating in the composite process. By further varying the number of atoms in each plane but keeping the ratio of participating atoms constant, jogs could be obtained in the traces and hence wavy slip lines could be produced. Vogel and Brick&apos; studied the behavior of a iron single crystals in which they suggest that the plane of glide is "non-crystallographic" and may be predicted from the intersection between the great circle joining the slip direction and specimen axis with the great circle whose zone axis is the slip direction. In a more recent investigation on iron single crystals, Steijn and Brick" suggest that the slip mechanism may be considered as made up of a type of composite slip occurring on {110} and {112} planes. Evidence for a possible composite nature of the slip process has been presented for the case of molybdenum in the form of analysis of asterism and specimen axis rotation." Definite proof of a composite slip process must, however, await good electron microscopic resolution of the individual traces making up the unresolved optical trace used in determining the acting slip plane. The present investigation was undertaken to study the behavior of columbium single crystals not only in tension but also in compression since the specimen axis migration should indicate the plane or planes of glide in the same manner that the specimen axis migration in tension indicates the direction of glide. The orientations of eleven crystals investigated are shown in Fig. 2. Specific orientations are missing (those in the vicinity of [Ill] and [001] and consequently the effect of orientation on the crystallography of deformation could not be considered. Experimental Procedure The 1/8 in. rods (7 in. long) were subjected to an axial tension in vacuo while at temperatures in the vicinity of 2000°C for 2 to 4 hr. This treatment resulted in large cylindrical grains (about ½ in. long) occupying the entire cross section. A number of these rods were used for the tension studies by observing the behavior of the individual grains. For the compression studies, single crystals approximately % in. long by 1/8 in. in diameter were cut from the rods; the ends were ground parallel. All specimens were polished electrolytically in a solution of 15 cc HF(48 pct) and 85 cc H2SO4 (concentrated) using a platinum cathode, a current density of 0.04 amp per sq cm and a temperature between 25" and 60°C.10 Orientations were obtained using a Laue back-reflection method (3 cm film to specimen distance) with a ½ mm collimator 9 cm long. For the compression specimens, a reference mark was scratched on one of the compression sur-

Jan 1, 1954

By Hisaaki Takata, Nobukazu Nanko, Ichiro Izawa

INTRODUCTION Tochibora Mine belonged to Kamioka Mines, which are located in Gifu Prefecture, the cen- tral part of the Japanese main island, has occupied the important position as a main source of silver, lead and zinc for the smelter of Mitsui Mining & Smelting Co., Ltd.. The annual production of crude ore goes up to about 1 mil- lion metric tons with average grades of 20g/t Ag. 0.31% Pb, and 4.18% Zn. For the last 20 years, the mine has struggled with the depressed zinc metal price in yen and the escalation of operating cost, especially la- bour cost. For instance, prices of commodities and labour cost have been raised 8 times and 14 times respectively during this period. On the other hand, total operating cost has been con- trolled to increase 4.5 times. The productivity of the mine has been increased 4 times by means of improvement of individual works and adoption of perfectly mechanized trackless mining system to reform the mining method. Some improvements are presented as follows; Today, drifting is carried out by the tunnelling crew which consists of 9 operators equipped with 5 Mobile-Jumbos, 2 LHD&apos;s and a jeep for carrying and loading ex- plosives. In order to get the high utilization of these machines, each crew manages systematically and continuously adjacent 15 faces under the direction of a forceman. As a result, we have accomplished high advance of drift. Furthermore, raising is carried out by a set of the raise-borer in case of long raises like ore- passes and also by the stage blasting method in case of short ones like slot-cuts. Generally speaking, the sublevel stoping method is considered to be one of the best methods for various respects; high productivity, low cost, easy grade control and safety. This method has been introduced in Tochibora Mine since 1950 and is now widely applied to lodes that could not be mined before by this method be- cause of the shapes of them and the conditions of their country rock. Now we are convinced to be nearly accomplished for our method. This report presents some examples of the standard sublevel stoping method and its variations which are practised at the mine. STANDARD SUBLEVEL STOPING Up to 1979 since 1950 when this method was first applied at the mine, 17 million tons of crude ore have been produced by this method, which amounted to 55% of the total production of the mine. During three decades, the productivity has been increased considerably by means of trackless mining system using large-sized machines and etc.. In other words, mining efficiency has been increased from 20 tons/man.shift to 100 tons/man.shift at large stopes. Formerly undercutting was carried out above the drawing drift by jack-legs and small scrapers and then several cone-shaped glory holes were made by stopers between the undercut level and the draw level. But now, a undercut drift is driven in parallel with the haulage drift at the same level of it. And at the undercut drift, drilling upward is carried out by a large-sized machines like the fan drill in order to extract the broken ore directly at the drawing drift connected with the haulage drift. Simplification of the work as well as utilization of large- sized machines enables to get higher productivity. But if the deposit is comparatively wider and the broken ore around the middle part of the deposit cannot be extracted, several drawing drifts are driven to the deposit and in order to minimize dead ore at the final stage of operation, the

Jan 1, 1981

By D. E. Norquist, J. E. Moeller

The results of wear on marked balls, 4, 31/2, 3, and 2 in. diam are given. All balls were forged steel of practically the same chemical analysis and hardness. The results indicate that balls in a given mill for a given length of time will have equal diameter losses, regardless of size. IN order to determine the relative wear rates of several sizes of grinding balls, groups of 4, 31/2, 3, and 2 in. balls were marked individually and were charged, all at the same time, into each of two production mills grinding copper ore. The remainder, and vast majority, of the ball charge consisted of 2 in. diam, and smaller, white, cast iron balls. The original weight of each test ball was determined and recorded. Some of each group of test balls were recovered from the mills periodically, individually reidentified, and reweighed. The test balls were recovered during regular maintenance shutdowns, at approximately thirty-day intervals, so as to avoid disrupting operations. As soon as the weights had been recorded, each marked ball was recharged into the mill from which it had been taken. The test units were mechanically the same and theoretically received equal tonnages of feed. All of the test balls were of forged, alloy steel composition with only slight variations in chemistry that would not be expected to affect the physical properties. All were heat treated in the same manner to produce a high hardness, as equal as possible for all sizes and as uniform as possible from surface to center. Generally speaking, the hardness of the portion worn from the balls during the test ranged from 62 to 65 Rockwell C. The microstructure was, therefore, predominately martensitic. The method of marking the test balls consisted of forming a small, round hole, 3/16 or 1/4 in. diam, into the center of each test ball with a Thomas Metal Master disintegrator, which produces a hole in fully hardened steel without affecting the hardness of the surrounding metal. After the hole was formed, each test ball was individually weighed to the nearest gram and the weight was recorded. The balls were grouped as to size and each group assigned a code letter. The individual balls within the various groups were then assigned a number. A small copper disc was stenciled on one side with the group letter and on the other side with the individual ball number and dropped into the hole in the corresponding test ball. The hole was then plugged with a low-melting-point metal alloy, which could be melted out in boiling water. Half of the test balls in each group were charged into one mill and the other half into another mill, so that all test balls in each mill would be subject to, as nearly as possible, identical conditions for an equal length of time. Previous testing had indicated that the wear rates on balls of different sizes could not be accurately compared if weight loss, or percentage weight loss, were used as a basis for comparison. Fig. 1 is a graphic record of the average weight loss for each size group in mill No. 1, and it becomes readily apparent that the larger balls lose substantially more weight in a given length of time. Fig. 2 is a graphic record of the average percentage weight loss for each size group in mill No. 1, illustrating that the smaller balls definitely lose a greater percentage of their original weight in a given length of time. It was, therefore, decided to convert the actual weights of the test balls to diameter and follow the diameter losses periodically to see if the wear rates

Jan 1, 1951