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By S. J. Hussey

This Bureau of Mines report presents a discussion of the statistical approach to the design of experiments and indicates, by concrete examples, how and when statistical design is essential for obtaining meaningful data with a minimum number of experiments. Every research worker plans his work and designs his experiments in a manner which, based on his experience, seems most rational to him and which he believes will produce the information essential for resolving the problems. If the results obtained are open to multiple interpretations and are not of definitive reliability, the failure of the experiment design to produce the desired information may be due to several causes, These include faulty judgment in selecting the factors to be tested, ignoring the importance of interaction between factors, failure to adequately control test variables, and assuming that meaningful trends in the results can be identified without comparison to a predetermined experimental error. An experienced researcher probably will deduce from the nature of the data obtained that the design is faulty and may by trial and error ultimately arrive at the correct solution to the problem. Statistical methods of planning research minimize the chance of faulty experiment design, embody concrete procedures for testing the validity and reliability of the test data and for indicating mandatory changes in the design, and enable the researcher to obtain meaningful information with the least number of tests.

Jan 1, 1963

By Earl L. Hastings

Although the principal market for diatomite in the United States is in the East,4 production of the material is presently restricted to the West, because the deposits are larger, mining costs are cheaper, and the quality of product is better than that obtained from other domestic deposits. However, Tallahatta diatomite, occurring in Choctaw and Clarke Counties, Ala., has a freight rate advantage, which should encourage competition for those market that are now being supplied with the purer diatomites from the western deposits. For this reason, diatomite occurrences in the Tallahatta formation were examined by the Bureau of Mines and physical properties of samples from the deposit were determined to obtain additional data for use by any potential producer who wished to evaluate the material for its commercial possibilities. In 1894 K. M. Cunningham5 found that the buhrstone formation (now known as the Tallahatta formation) contained "siliceous shells of marine diatoms, radiolaria and foraminifera, thus being rather of the nature of tripoli or diatomaceous earth than of a true clay." Cooke6 and Semmes7 also reported the Tallahatta formation to be composed principally of diatomaceous earth with accompanying beds of sand, clay, and sandstone.

Jan 1, 1963

By Ruth F. Brinkley

Principle activities of the Bureau of Mines Explosives Research Laboratory from July 1, 1960 to June 30, 1961 are reviewed briefly in Part 1. Part 1 also includes data obtained in connection with several minor investigations which are not sufficient to warrant separate publications. Part 2 gives brief abstracts of publications that appeared during fiscal year 1961; in general, the research reported in these publications antedates this period.

Jan 1, 1963

By G. T. Krempasky

This report covers the installation and evaluation of lb reinforced concrete sets, 6 in each of 3 mines in the Goeur d'Alene mining district, Shoshone County, Idaho, and is the second of a series to determine the feasibility of a more permanent type of mine support. Closure measurements, where applicable, were made periodically of the concrete-set installations and were compared to the initial cross section of the sets. A different method of blocking was used at each test site; at one test site the type of blocking was changed several times during the test. Results from each test site are reported separately. No attempt was made to compare the cost of the concrete installations with the cost of other types of support used in the district. Such an evaluation of permanent types of support would require a longer period of time. At this time, tests are not complete enough to determine the applicability of underground concrete supports. However, results to date tend to confirm the general opinion that precast concrete mine supports could be used to advantage in openings that require support and must have long life, especially where decay of timber is an important factor.

Jan 1, 1963

By Robert Charles Alfred

Evolution is continuing in the field of rock drilling, Campbell Limestone Company is experimenting in the higher air pressure phase of drilling, It has been determined that there is a definite relationship between Air Pressure, Penetration Rate, Bit & Tool Wear and Life, In our drilling we have determined that &e higher air pressure gives a better penetration rate with less bit wear per foot. Drilling with 180 to 200 PSI air pressure, instead of 100 PSI for air and/or churn drills, has decreased our primary costs by approximately one half.

Jan 1, 1963

By Bunting S. Crocker

This paper reviews the trends in the past two years in autogenous grinding throughout the world. It covers rock grinding in South Africa, Sweden, Canada, the United States, Finland and Germany. To properly orient the discussion on this subject, the paper attempts to define and classify the scope of autogenous comminution. As this is a relatively new subject, there is often considerable confusion regarding the various practices, which sometimes differ widely. By clarifying the types and forms, we hope to help clear up this con-fusion. Autogenous grinding is being carried out, throughout the world, either in mills grinding in water or solution or in dry mills using air classification to remove the finished material. The wet grinding, particularly, can be divided into: (1) (2) (3) Primary autogenous grinding, or "run-of-mine" grinding. Secondary autogenous grinding or semi-autogenous grinding or rock pebble grinding. Combination processes. -This covers plants in which pebbles made in the primary mill are re-moved and used as grinding media for fine grinding in secondary mills.

Jan 1, 1963

By F. Taylor Ostrander

Some countries are infinitely poorer than others in mineral resources-despite the perfect equality of their political leaders ambitions. Compare the mineral poverty of Kenya and Tanganyika with the riches of Katanga Province and Northern Rhodesia. Compare Paraguay with Chile, There never has been any equality in the distribution of nature's wealth. Minerals cannot play any role at all in economic development where they don't exist, and there are bound to be differential rates of economic development where there are basic differences in the wealth of mineral resources available. Africa is my principal area of interest and I know that there is an unfortunate but widespread misconception about Africa's "vast mineral resources, "its "untapped mineral wealth." Why is it untapped? Why is it undeveloped?

Jan 1, 1963

By G M. Young

IT IS most appropriate that this first Memorial Lecture should be given in the Province of Quebec, near the site of the first metallurgical industry in Canada. At La Forge, about seven miles north of Three Rivers, iron was produced in 1783. We are told that the early settlers obtained most of their iron-ware -stoves, kettles, axes and ploughshares -from this smelter, with its foundry and forge. The Canadian copper industry also had its beginnings in Quebec when, nearly 100 years later, in the 1880's, several small copper smelters were erected in the Eastern Townships. Later, in 1899, Canada's first aluminum smelter was built at Shawinigan. From these small beginnings has grown a vast metals industry, the export value of its products being only exceeded by that of our forest products -newsprint, pulp-wood and lumber. As we are not a large country in terms of population, our domestic capacity to consume is often small in relation to our developed capacity to produce.

Jan 1, 1963

By J B. McConnell

The Thompson smelter has three unique features which form the basis ~f its design: fluid bed roasters which treat nickel concentrate filter cake from the mill, as well as the flux, in order to achieve partial desulphurization; the use of electric furnaces for the smelting of the partially desulphurized, preheated roaster product; and the disposal of slag by water granulation and slag slurry pumping. The installation consists of three fluid bed roasters, each feeding an electric furnace. Nickel concentrate is received at the smelter via pipe line. It is thickened and filtered, and the filter cake, together with siliceous flux, is fed through rotary bin feeders and reciprocating double-gate seals into the fluid bed roasters. Air injected into the roasters through club-head tuyeres oxidizes part of the sulphur and associated iron in the concentrate. The heat of reaction dries and heats the charge. Roaster product is recovered from the gas stream in cyclones and from the roaster bed through automatic valves.

Jan 1, 1963

By T. A. Henrie

A technique was devised for measuring the rate of chemical reactions between reactive metals and molten-salt mixtures at high temperatures. The rate of the heterogeneous reaction between high-purity titanium metal and titanium trichloride in molten sodium chloride was determined. The reaction is surface-controlled, and the heat of activation is 8.29 kilocalories per mole TiC13. An active site or reaction nuclei is created by adsorbing a TiC13 molecule at the metal surface. Reaction of the second TiC13 species forms an activated complex that decomposes into three TiC12 molecules.

Jan 1, 1963

By Ruth F. Brinkley

Principle activities of the Bureau of Mines Explosives Research Laboratory from July 1, 1960 to June 30, 1961 are reviewed briefly in Part 1. Part 1 also includes data obtained in connect ion with several minor investigations which are not sufficient to warrant separate publications. Part 2 gives brief abstracts of publications that appeared during fiscal year 1961; in general, the research reported in these publications antedates this period.

Jan 1, 1963

By J M. Fletcher

The responsibility and scope of the Industrial Engineering Department, as organized at the Jeffrey mine, has been broadened to include any study, project or report that could result in more effective use of men, materials and equipment. Although still emphasizing wage incentives and co t reduction, much more varied work is now done, consistent with the in-.creased complexity of industry. Additional activities now include production, maintenance and inventory control improved job evaluation, packaging, labour utilization studies, technical sales liaison, mining, milling and service department n1ethods, plant layout, and specialized project analysis. Additional techniques include the extensive use of work .sampling and standard data. A recent trend has been toward increased emphasis on industrial relations, both in introducing change to the men and in providing requested explanations to Union stewards and officers. These new responsibilities have resulted in the development of specialists in some rather narrow industrial engineering fields, as well as the necessity for industrial engineering assistance in supervisory and job training.

Jan 1, 1963

By Raymond L. Carpenter

The thermal conductivity, electrical resistivity, and Seebeck coefficient for nine compounds, based on the formula for enargite Cu3AsS3, were measured in a search for efficient materials to be used in thermoelectric generators or refrigerators. Results indicate that one of these compounds, Cu3SbSe4, has thermoelectric properties approaching those of bismuth telluride. An investigation of the effect of adding small quantities of tellurium to Cu3SbSe4 and Cu3SbS4 in order to improve their properties also was made. A figure of merit of 2.1 x 10-4 °C-1 was obtained for Cu3SbSe4 + 0.1 percent tellurium.

Jan 1, 1963

By Albert W. Deurbrouck

This report describes the preparation characteristics of the significant, presently producing coalbeds in Mercer County, W. Va. Approximately 650,000 tons of coal was produced in Mercer County, W. Va., in 1960, of which over 630,000 tons was cleaned in four preparation plants. In 1960 the Pocahontas Nos. 3, 6, and 11 coalbeds supplied 99.5 percent of the total coal mined in the county. Because the number of working mines In this county was small, only six samples were collected; four of which were of metallurgical quality as mined. The remaining two samples could be upgraded by washing at suitable specific gravities. Many of the samples taken were of metallurgical quality as mined; however, the float-and-sink analysis on these coals has been included to point out their amenability to the production of premium quality, special purpose coals. In general the coals were low-volatile bituminous in rank with low ash and sulfur contents.

Jan 1, 1963

By E. Hornbogen

Discontinuous precipitation in a iron can occur by at least two different mechanisms. These mechanisms are compared, using observations made on an Fe-22 at. pct Zn alloy and an Fe-19.5 at. pct Mo alloy. In the Fe-Zn alloy, precipitation began on grain boundaries. These boundaries moved into the supersaturated solid solution, providing nucleation sites and an easy path for diffusion. The precipitated phase pew as lamellae, perpendicular to the PRECIPITATION reactions are called discontinuous if the nucleation of particles does not occur on individual sites in the supersaturated matrix.' In discontinuous precipitation, nucleation and growth occur on a reaction front that moves into the supersaturated solution and leaves a two-phase aggregate behind. The term cellular precipitation2 has also been used, but the term autocatalytic precipi- moving reaction front. The orientation of the depleted iron differed from that of the supersaturated iron. In the Fe-Mo alloy the growing precipitate particles apparently created dislocations in the growth front which served as nucleation sites. The precipitate grew on (110) planes of the iron, and growth occurred through volume diffision. The depleted iron retained the orientation of the supersaturated solid solution. tation seems to describe the nature of such reactions best. The basic effect of such a precipitation mechanism in a solid is that it is able to move or create sites that can catalyze nucleation. Such sites can be grain boundaries and dislocations. A mechanism of autocatalytic precipitation must, therefore, include some rational process by which a grain boundary may move into the supersaturated matrix or by which dislocations may be generated in front of the reaction. Discontinuous precipitation is always in competition with individual nucleation and growth of par-

Jan 1, 1963

By Carl Rampacek

The conversion of dilute sulfur dioxide gas into sulfuric acid by autoxidation in mechanical cells of the flotation or gas absorber types was investigated. Bench-scale tests were made with sulfur dioxide-air mixtures to determine the influence of several factors on autoxidation of sulfur dioxide, using iron and manganese salts as catalysts. The laboratory investigation subsequently was extended to pilot plant acid-making tests, using a modified turbomixer gas absorber having a 12-inch-diameter impeller. Sulfur dioxide gas was produced for the tests by roasting pyrite in a fluidized-bed reactor. In the better tests, made with manganese sulfate as the catalyst, the equivalent of 1,000 pounds of anhydrous H2SO4 was produced per 24 hours as a 10-percent solution; power consumption was 0.2 kwhr per pound of equivalent anhydrous acid synthesized. The batch and continuous tests demonstrated the technical feasibility of producing dilute sulfuric acid by autoxidation of sulfur dioxide gas in mechanical cells when converting pyrite roaster or waste smelter gases.

Jan 1, 1963

By G. S. Tint, M. Herman, V. V. Damiano

Dislocation arrays and substructures were studied in cadmium doped zinc crystals using a newly devised etching technique. Cadmium precipitates delineating the dislocations were revealed by etching a surface closely parallel to the (0001) slip plane. Cinephotomicrography of the continuous etching process revealed the three-dimensional aspects of dislocations in the bulk crystal. Dislocation etch patterns were studied in both deformed and annealed crystals after suitable aging at room temperature. The effect of annealing was evidenced by a rearrangement of the dislocations into low-angle boundaries and hexagonal networks. ETCH pit techniques have been used extensively to study dislocations in both deformed and annealed bulk metal crystals. Ideally one hopes to obtain a one-to-one correspondence between the etch pits and the points of emergence of the dislocations at the surface. One then attempts to deduce the way in which dislocations are arranged in the bulk crystal from the arrangement of etch pits on the surface. It is clear that one can obtain only limited information of the dislocation configurations inside the crystal from etch pit studies of single surfaces. Considerably more information is obtained if one is able to follow the course of the dislocations through the crystal using progressive etching technique. Techniques of this sort were used by Gilmanl to study dislocations on the slip planes of NaCl crystals and by Damiano and Tint2 to study dislocation arrangement in zinc crystals grown from the melt. The present paper makes use of a technique first described by Tint and Damiano3 to observe and continuously record the dislocation structures which appear while a crystal surface was being progressively etched. Studies were made on cleaved (0001) surfaces to reveal the dislocations along their length on the surface closely parallel to the slip plane. The technique for revealing segments of dislocations along their length by etching is well known. Wilsdorf and Kuhlmann-wilsdorf4 revealed disloca- tions along their length in aluminum containing a few percent copper, when precipitates segregated along the dislocations. The technique was used by Low and Guard5 to study dislocation configurations on the slip plane in Fe-Si alloys containing carbon. In the present work the technique was applied to zinc containing cadmium since it was shown by Gil-man6 that a cadmium-rich phase could be made to precipitate from supersaturated solutions along dislocations in zinc. Segments of dislocations delineated by the precipitates were revealed by etching a surface prepared by cleaving the crystal. The three-dimensional nature of dislocations and substructures was thus studied from the cinephotomicro-graphic record of the continuous etching process. EXPERIMENTAL Single crystals of zinc containing the order of 0.1 pct Cd were prepared by slowly lowering a graphite crucible containing the melt through a temperature gradient of 15°C per cm at a rate of 1.5 X 10-3 cm per sec. "As grown" crystals were aged for periods of 1 month at room temperature, then cleaved in liquid nitrogen, and etched according to the procedure used by Gilman.' The etchant containing 32 g of CrO3, 6 g of hydrated Na2SO3 in 100 ml of water behaved as a chemical polish for zinc and etch pits were produced at the site of precipitates or inclusions. After the precipitates or inclusions were removed from the surface, the etch pits left behind were eventually polished smooth. This behavior enabled one to continuously observe the surface while the specimen was immersed in the etchant. Best results were obtained when the specimen surface was vertical and the reaction products of polishing were continuously removed by gravitational convection. Some crystals were heavily deformed in excess of 25 pct strain, others were lightly deformed the order of a few pct by compression such that the deformation occurred essentially by basal glide. Some crystals were etched immediately after deformation, others were allowed to age at room temperature for several weeks prior to etching. Heavily deformed crystals were annealed at various temperatures and etched on the cleavage plane immediately after annealing, others were allowed to age at room temperature for several weeks prior to etching. The etched structures of deformed and annealed structures were studied. Similar experiments were conducted on 99.9999 pct pure zone refined Tadanac zinc crystals which

Jan 1, 1963

By P. A. Wasson

The investigation described in this publication was conducted by the Bureau of Mines to determine the effectiveness of the anionic silica flotation method on goethitic iron-bearing materials from the Cuyuna Range, Minn. Samples used in this investigation were a composite of drill core from 13 holes, and 3 samples from lean ore stockpiles. These samples are believed to be typical of the mineralization occurring in an area with a potential reserve of several million tans of submarginal iron ore. Results from batch tests showed that the iron-bearing minerals could be effectively concentrated by flotation removal of the siliceous gangue. The drill hole composite yielded laboratory flotation concentrates from locked tests containing 56.8 percent Fe and 6.1 percent silica, with an accompanying iron unit recovery of 94.2 percent. Concentrates containing 52.4 to 53.7 percent Fe also were produced from the lean ore stockpile materials; corresponging iron recoveries ranged from 71 to 79 percent in the batch tests, with the possibility remaining for additional recovery of iron from the middlings.

Jan 1, 1963

Most mines in the Bundamba, North Ipswich, and Rosewood districts of the West Moreton coalfield of south eastern Queensland have installed washing plants during the last five years. Many problems were encountered in their installation, including the small size of washing plant required in many cases, the economical minimum ash content under present and future market requirements, production from a one-product washbox of large and small coal of quality to satisfy both markets, measures to avoid adding unnecessary moisture to the washed slack coals, and excessive middlings in some coals or soft clay in others.INTRODUCTIONIt was fortunate for Brisbane, which was to become the capital of a new State, Queensland, in 1859, and grow into a city of over half a million people by the time of its centenary, that coal was found in abundance almost on its doorstep near Ipswich, the first mine being opened at Redbank in 1843. This was followed by the opening of many more mines in that district and, some 40 years later, in the nearby Rosewood district where high-volatile gas coal was produced (Fig. 1). These discoveries ensured a supply of reasonably priced coal (currently about 85/- per ton delivered) in Brisbane, but the quality is inferior to that of other coals mined in Queensland beyond economic range of Brisbane.Various factors led to an increase in the average ash content of the West Moreton coals during and after the war. Between 1940 and 1952 the gasworks coals rose in average ash from 13 8 per cent to 23·9 per cent and the powerhouse coals from 17·1 per cent to 27·1 per cent. This drift was arrested by the installation of 28 screening and picking plants from 1952 onward, but it became obvious that mechanical cleaning of the coals was essential due to the competitive market for coal and the worsening quality of reserves.

Jan 1, 1963

By C. L. Coldren

Recently there has been much discussion of the use of pipelines for the long-distance transportation of solids. Many have come to recognize the economies inherent in pipeline transportation. The widespread movement of oil and gas at astonishingly low costs - a gallon of oil moves from Montana to New York for less than that for the delivery of a postcard - has spurred others to sturdy this mode of transportation. Most interested people are aware of the inherent advantages of pipelines - continuity and reliability of operations - low manpower requirements per ton mile - moderate capital costs per ton mile - low maintenance costs per ton mile - low operating costs per ton mile.

Jan 1, 1963