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COLUMBIA SECTION STANLY A. EASTON, Chairman, FREDERIC KEFFER, Vice-Chairman, L. K. ARMSTRONG, Secretary-Treasurer, P. 0. Drawer 2154, Spokane, Wash. D. C. LIVINGSTON FRANK A. Ross The first meeting of the Columbia Section was held on March 24, as a part of the 1916 Northwest Mining Convention which was held under the -auspices of the Spokane Mining Men's Club assisted by the Spokane Chamber of Commerce, the technical program being in charge of the Spokane Engineering and Technical Association assisted by the local sections of the A. I. E. E., A. S. C. E., and A. I. M. E. The program of the successive sessions was carefully arranged with view to its application to mining, and in addition to the technical program there were exhibits of ores, minerals, devices, etc., of interest to the delegates, who numbered over 500. A portion of the program was also arranged with special reference to the requirements of the prospector and miner. A reception, a banquet, a complimentary luncheon, a regular daily call' of the Stock Exchange, a visit to the High Schools and to one of the substations of the Washington Water Power Company and to the Union Iron Works kept the visitors entertained, the ladies being looked after by a special committee of ladies who held open house during the entire week. Several important resolutions were passed by the Convention and one by the Columbia Section, A. 1. M. E. With Stanly A. Easton, chairman, presiding, the Columbia Section, American Institute of Mining Engineers, occupied the time between 2.00 and 5.30 p.m., March 24th, the Moorish room of the Spokane hotel being filled with members and their guests. "The Apex Law and the Mineral Surveyor" was a paper presented by F. W. Callaway and generally dis-cussed because of its local application in the Coeur d'Alenes, the conclusions being reached after expensive litigation between two of the large mining operators in that district.

Jan 6, 1916

By D. Houghton

"I am very pleased to be a member on this panel today because abrasion and wear in mills has been part of my life over the past forty years. My presentation will deal with the role Ni-Hard has played in combating wear and abrasion in mills. Before Ni-Hard came along, unalloyed white iron was used in ball mills and one of the most popular types of white iron liners was the pocket liner. Slide #1 illustrates the design of the pocket liner used at Dome Mines in their 5' x 22' pebble mills. The pockets filled with grinding media and it was on this that the wear took place. The concept is not unlike the new magnetic liner which utilizes the ore and grinding media to form the wearing surface. In this slide please note the tapered pocket type of cored bolt holes. If cored bolt holes do not fill with grinding media there could be excessive grooving or wear at that area. Therefore all cored bolt holes should be tapered in this manner.Before Inco patented the name Ni-Hard several foundries were making the alloy iron under different brand names such as Diamond Alloy, Mitchelloy and Specialloy. In the early days some of the Ni-Hard was poor quality. Inco provided foundries with technical knowhow and provided assistance to licence them to sell under the name of Ni-Hard. This was in the late 1920's. The material we are discussing is Ni-Hard type I with the following analysis (slide #2). It is a martensitic white iron with BHN of 550 - 600 and is a relatively easy alloy to produce in either a cupola or electric furnace. The annual average production of Ni-Hard in North America is 90,000 tons with mill liners making up 25,000 tons and grinding media 30,000 tons, according to Warren Spear of Inco."

Jan 1, 1983

By Peter Moser

The average annual consumption of raw minerals in Europe is 10 ton per person. About 50 % is produced by blasting. For a population of 450 million (including the population from the countries of the new member states) this makes 2.25 billion tons of blasted rock, 80 % being building industry aggregates and industrial minerals. In aggregate quarries 10-15 % of the rock blasted can’t be sold, as the material is too fine, i.e. smaller than 4 mm. This ‘fines problem’ is worse in the quarries of limestone and cement producers where up to 30 % of the material is useless. Thus about 450 million tons of useless rock fines are produced and put on waste dumps every year, i.e. 1 ton/person. This problem is addressed by the research project LESS FINES - “Less Fines production in aggregate and industrial minerals industry” which is funded by the European Union under the project contract G1RD-CT-2000-00438. The project consortium, formed of nine partners from 5 EU countries, works on the following two main research subjects: 1. The determination of the natural breakage behavior (NBC) of the rock mass, which is defined as the particle size distribution curve for a certain rock mass with the maximum uniformity and thus for a given maximum particle size that fragmentation curve which gives the minimum amount of unusable fine material. The comparison between the NBC and an actual blast fragmentation curve allows to quantify the fines reduction potential. 2. The adaptation of explosives properties, charging techniques and timing in order to produce only the minimum, inherently unavoidable percentage of fines. With about 15 full time working persons the project is estimated to be one of the largest blast related research activities in Europe at the time of the project period. The project is coordinated by the Department of Mining Engineering& Mineral Economics of the University of Leoben.

Jan 1, 2004

By Dan Plazak

Discussion by Dan Plazak The authors are to be congratulated for presenting a simple and practical tool for quick estimates of ground water flow rates. At the risk of detracting from the simplicity of the method, I would like to suggest a slight refinement to the equation as presented. As the authors noted, the Jacob-Lohman equation (1952) assumes confined-aquifer conditions. To use confined-aquifer equations in water-table aquifers, Jacob (1963) presented a correction to convert water-table aquifer drawdowns [Ahw] to equivalent confined aquifer drawdowns [Ah,: 2] [Ah Ah = Ah - w(1) Cw 2H where: Ah, = Drawdown in confined aquifer: Ahw = Drawdown in water-table aquifer and H = Original saturated thickness of aquifer] Substituting the above in equation ( I) of Hanna. Azrag and Atkinson [4nT Ah - 2H ) Qj2.25 T t(2) 1 nr2 S W] Since the above expression predicts lower pump rates, it causes the Jacob-Lohman equation to agree more closely with appropriate analytical and numerical models. Figure 1, adapted from Fig. 5 of Hanna. Azrag and Atkinson, illustrates the closer agreement of the modified equation to their numerical model, as reflected in Qm/QJL ratios closer to unity. The agreement improves particularly as drawdown [Ah] becomes large in relation to aquifer thickness H. An additional advantage of the modified equation is that Hanna, Azrag and Atkinson's correction factor C is much more stable as pit depth increases. Assuming, as did Hanna, Azrag and Atkinson, that their numerical model is an accurate predictor, it is clear that the modification incorporated in equation (2) improves the accuracy of preliminary estimates of ground water flow to a pit.[ ] References Jacob, C.E and Lohman. S. W.. 1952, "Nonsteady flow to a well of constant drawdown in an extensive aquifer." Transactions, American Geophysical Union. Vol, 33, No. 4. pp. 559-569. Jacob. C. E.. 1963, `Determining the permeability of water-table aquifers,' USGS Water-Supply Paper 1536-1, pp. 245-271

Jan 1, 1995

By C. G. Dunn, F. Lionetti

W. G. BURGERS*—It seems almost certain that this investigation shows the way which finally, when more analogous data have been obtained, must lead to the understanding of many features of preferential growth-directions of crystals and of the occurrence of recrystallization textures. In this connection I should like to mention that Mr. Tiedema in my laboratory succeeded in developing an analogous method for preparing crystals in aluminum plates with a chosen crystal-lographic plane and direction parallel to the surface of the plate (to be published in Cryst. Ada). If such crystals were grown in high purity aluminum and test-pieces containing a few crystals such as the authors describe were prepared for this metal, it might be possible that due to the absence of growth obstructing particles, even in this low-melting point metal boundary displacements approaching equilibrium positions might be realized. With regard to the apparently marked drop in surface energy for orientation differences approaching zero degree, and orientation differences approaching those existing between twins, it seems of interest to remark that in aluminum a crystal growing at the expense of fine grained material cannot (or can only very reluctantly) absorb grains in either ap- proximately (within 5—10°) parallel or spinel twin orientation (May, Tiedema and Burgers, Nature (1948) 162, 740 and Cryst. Ada in press). Consequently with aluminum the method of preparing a crystal with a definite orientation does not succeed when the new crystal has to absorb its own texture; for example it is not possible to grow in a polycrystalline wire with a [lll]-texture a crystal with a [11 Indirection parallel to the wire axis (Tiedema: Cryst. Ada, in press). Finally I should like to mention the well-known fact (Burgers: Proc. Acad. Amsterdam (1947) 50, 723) that prolonged annealing of recrystallized nickel-iron sheet with cube-texture never succeeds in transforming this into one single crystal of the same orientation; if, by "secondary re-crystallization," large crystals are formed

Jan 1, 1950

F. G. SMITH, Waterbury, Conn.-I would like to ask whether small amounts of iron give the maximum resistance at a low temperature, and if the large amounts of iron raise the temperature at which the maximum resistance occurs? That is, with a small amount of iron, will a maximum be at, say, 10°? F. E. BASH.-With the small amount of iron, the maximum is at a lower temperature, and with the increase of iron, the maximum increases; it seems to come to a maximum and then decrease; that is, increasing the iron up to a certain value increases the temperature at which there is a maximum of resistance, and any increase of iron beyond that value will start decreasing this temperature. With 2 per cent. of iron, the maximum is lower than for 1.5 per cent. which was the value that we found to be satisfactory. F. L. DRIVER,* Jr., Harrison, N. J.-I would like to ask what chance there is of the instrument companies getting together and deciding on standards for both manganin and constantan? We make both of these alloys in this country and we find that each one of the instrument com-panies who buy these materials require different standards of specific electrical resistance and thermal e.m.f. For instance, some of our cus-tomers require an electrical resistance in manganin or therlo of 240 ohms per circular mil foot and others require it with a specific electrical resist-ance of 270 ohms per circular mil foot. They buy these alloys in relatively small quantities so that it means much extra melting and supervision when making up small quantities for each consumer. If something could be. clone to eliminate this, it would be a benefit to the instrument com-panies, who could secure their material more cheaply, and to the manu-facturers, who would not have to spend so much time and effort in special manufacturing.

Jan 12, 1919

By Bryan Wilson

Background ?Nickel Rim South Mine started production ramp-up in Q2, 2009. ?The main dewatering pumps were put into use in August 2009. ?3 Feluwa?multisafe?positive displacement pumps ?1700m single lift pumping ?Reliability has been an issue due to the amount of slimes and fibers (from shotcrete) at the pumps. ?Critiqued internal dewatering system to solve some issues we were having with our sumps Findings 1.Much of the final dewatering system was not in place. a)Temporary pain. Difficult to say something is not working when the system was not yet in place as per design. b)Not enough capacity to handle slimes within the system. 2.Need to address issues with the final design: a)Ongoing costs: The end design has operating costs of $2.5 million b)Scoops in Sumps: The end design relies on scoops to be used for cleaning the sumps c)Slimes Recovery: The system mixes 3 different products in the sumps along with the fibers d)Pump repair costs: The existing Tsurumi pumps are too light duty for our slimes

Nov 1, 2011

By S. Neven

The smelting of copper anode slimes, a material which contains mostly lead, silver, copper and selenium, has been practiced for many years with a view to recovering the silver and associated small amounts of gold. However, a theoretical understanding of the process has been lacking and this handicaps efforts to improve and intensify smelting operations. In the past few years work has been done in this area and this work will be reviewed in the paper. The underlying thermodynamics of the oxidation of silver-copper selenide mattes has been developed and used as a basis for the construction of a computational thermodynamics model which attempts to predict the composition of all condensed phases during the course of smelting. The model will be outlined and its successes in matching experimental data, as well as its current deficiencies, will be considered. Supporting work on the thermodynamics of silver solubility in slags, on activity-composition relationships in the Ag-Se system and work in progress on the oxidation state of copper in the slags will be reviewed. These projects are designed to provide further detailed data which will improve the robustness of the thermodynamic model.

Jan 1, 1999

By Scott L. Burrill

In the past 100 years in the mining industry, many references are made to the "Widow Makers", 'Miners Con" and many other derogatory names related to physical hazards. They reflect the lack of understanding of the problem facing the early day miner. Workers were enticed, in some cases, to take a chance against a medical question mark that could not be explained by the doctors of those early days. The optimism of the mining man and the challenge of work led him to believe that the physical results could not apply to himself and only applied to some of his fellow workers. Much of the time, to his dismay, he found that he had lost to the game of chance. As medical knowledge improved and mining management began to understand the effects of conditions in the mines and beneficiation plants, steps were taken to alleviate or eliminate the health hazards that were present, The organizations engaged in mining that did not take an active interest in employee health found themselves to eventually be placed in the position of being forced to take action by Federal and State legislation. We find ourselves in the 1970's on the threshold of a new era where the general public is concerned vociferously about "their" environment and the industry feels the governmental controls more strongly than ever before. It can be said that in the past 100 years we have advanced from the "Widow Makers" of the 1870's to the "Retirement Makers" of today. The difficulties of the early days in underground mining were of times compounded in the beneficiation plants above ground. As late as the 1950's some crushing and milling installations in the United States were operating under environmental conditions that complied to the then existing legislation but were below the health level sought by conscientious management. The Mission Concentrator Crushing Plant was designed in 1959 and placed in operation in July, 1961. In the past ten years the crushing plant has been continuously complimented by technical people, government inspectors and casual

Jan 1, 1971

By C. O. Swanson

THE purpose of this paper is to discuss the use of the dip needle in the field of mining geology. The subject matter is new only to the extent that it reflects the writer' s added experience in recent years. The treatment is brief, and those interested in a more extended analysis are referred to the articles listed at the end of the paper. In the discovery and tracing of mineral deposits, the clip needle, like most other geophysical instruments, can be used in two ways. One method may be termed direct; the other, indirect. The direct method is that of finding or following certain ore-bodies by virtue of their magnetic properties. Explicitly, or by inference, it is the method which many mining men and practising geophysicists have in mind when they consider whether or not a certain property should be studied by geophysical means. In the ideal case, this method demands little or no knowledge of geological conditions. The indirect method uses the clip needle as an aid to purely geological studies in working out the structure of a mineralized area. Although not as simple as the direct method, it enjoys a much wider field of usefulness. The writer's experience in the past fifteen years, which is believed to be typical, is that the indirect method finds application four or five times as often as the direct method. The indirect method is of particular value because it furnishes information concerning the relationship between geological structure and ore occurrence. Most mining engineers will agree that structural control is an important factor in the localization of ore deposits, and therefore that the subject under consideration is of some interest in mining geology. Specifically, then, the present purpose is to outline the principles and practice of using the clip needle in working? out geological structure.

Jan 1, 1941

By D. W. Bridges, S. R. Borrowman

Thorium and yttrium oxides were recovered from siliceous ores of the Powderhorn , Colo . , area . Processing comprised ( 1 ) acid curing and subsequent ( 2 ) acid baking , ( 3 ) leaching , and ( 4) solvent extraction of thorium , using a primary alkylamine , and yttrium , using di - 2 - ethylhexyl phosphoric acid . About 95 pct of the contained thorium and yttrium was recovered from ore containing 1.2 pct Th02 and 0.5 pct Y₂ 03. The thoria product was 99 pct Tho ; the yttria product was 77 pct Y₂ 03. A 150 - to - 1 concentration ratio was effected on the latter , but some contaminating lanthanon - group oxides remained .

Jan 1, 1964

By S. E. Khalafalla

The Bureau of Mines investigated variations in the activation energy for the carbon monoxide reduction of magnetite and ferrous oxide with respect to the state of aggregation of the oxide material. Reduction phenomena can only be satisfactorily explained by including an adsorption step in the reduction process. Summation of the values of the exothermic heat of chemisorption and the variable apparent activation energy for reduction yields a nearly constant value of about 50 kcal for either ferrous oxide or magnetite regardless of whether they are aggregated in pelletized form or coarsely crystalline particles.

Jan 1, 1965

By Jonq-Keh Lee

This paper deals with the effects of air leakage from intake to return airways through a series of stoppings on the analysis of coal mine ventilation. The mathematical model which assumes continuous leakage along adjoining intake and return airways is reviewed, and a new mathematical approach is presented based upon the concentrated leakage through individual stoppings. The procedure incorporating the new method in the analysis of coal mine ventilation networks is also discussed.

Jan 1, 1984

By C. W. Owings

"PURPOSE OF REPORTThe safety and efficacy of permissible storage—battery gathering locomotives are becoming recognized more and more in coal mines. The great mobility of this type of haulage equipment is due to the fact that no trolley wire and bonding of rails are needed; hence wherever there is track and adequate ventilation to dilute properly any dangerous gases, the storage—battery gathering locomotive may go. As coal near the outcrop or the surface is mined out, coal farther from the outcrop or deeper in the ground must be mined, and gassiness of the coal bed often increases under these conditions. The use of electrical equip¬ment capable of giving off arcs or sparks while operating near or at the coal faces constitutes a serious explosion hazard. Often, it is uneconomical or impracticable to use animal haulage, and locomotives must be employed. The operator should consider the safest and most economical unit; permissible equipment is the answer to this problem, and storage—battery locomotives are the only permissible electric haulage units.A comparison of permissible storage—battery locomotives with cable—reel locomotives of the latest enclosed ""explosion—tested"" type has been made at the Keystone No. 1 mine of the Houston Collieries Co., at Keys one, W. Va. The information and data contained in this publication were obtained by the writer during an inspection of haulage at this mine.ACKNOWLEDGMENTSThe writer is indebted to P. C. Thomas, vice president and general manager, the Koppers Coal Co., operator of the Keystone mines, who granted permission for making the study. W. A. Wilson, general superintendent, Houston Collieries Co., arranged for the investigation and for obtaining the data. C. E. Zuspan, chief electrical inspector, and J. C. Newman, division electrical inspector, accompanied the writer underground and assisted materially in obtaining information and data upon the haulage methods and performance of the locomotives. The assistance or general mine Foreman Pierman and of mine foreman White is gratefully acknowledged."

Aug 1, 1931

By Sergey Dyachenko

"Following the adopted strategy for making the production modern, efficient and environmental friendly the Company completed a stage of the integrated program aimed at reconfiguration of its processing capacity.Upgrade of the Talnakh Concentrator with commissioning of two start-up facilities (SF) allowed an increase of 30% in its ore processing capacity up to 10 mtpa. In addition to a new high-tech equipment installed, a new concentration process was adopted offering the main advantage of 25-30% reduction of sulfides in concentrate. New concentration technology enabled the total amount of produced nickel concentrates (from Norilsk and Talnakh Concentrators) to be processed at upgraded smelting facilities of Nadezhda Metallurgical Plant and allowed decommissioning of smelting capacities of Nickel Plant resulting in emissions reduction by 30%.Nornickel plans to boost the capacity of Talnakh Concentrator to 18 mtpa by 2022, after commissioning of the 3rd SF. This will provide a shorter route for ores transportation from Talnakh mines along with improvement of cost/performance ratio of ore processing through the usage of the modern equipment and optimized concentration flow scheme. Total capacity of Talnakh Concentrator will be sufficient to process ores from Talnakh deposits with planned upstream assets development taken into account. Volume of ore mined from Norilsk deposits to be processed at Norilsk Concentrator will be also increased.Upgrading the crushing section at Kola MMC Concentrator in 2015 provided finer particles of the crushed ore, resulting in 6.6% increase in specific capacity of ore mills as well as 1% higher recovery of non-ferrous metals due to improved liberation of ore minerals.In 2015-2017 the Company was actively engaged in optimization of existing process flow schemes and parameters of Kola MMC, new high-performance reagents were adopted for concentration process, namely, collectors, depressors, flocculants. These measures allowed the Concentrator to reduce its annual operating unit costs and ensure sustainable production of concentrate with the lower grade of the incoming feedstock.Launched in October 2017, Bystrinsky GOK’s Concentrator was 3D designed and received a range of advanced technological solutions.All design process procedures and technologies rolled-out at the Company’s concentrators were developed by Russian R&D institutes, with the key role of Gipronickel Institute, R&D Service of Kola MMC and Polar Division's in-house Engineering Support Centre."

Jan 1, 2018

By M. Yamine, R. J. Ring, D. J. Waters

"An experimental program has been carried out by the Australian Atomic Energy Commission to compare the effectiveness of Caro's acid as an alternative oxidant to pyrolusite in the leaching of uranium ores from the Alligator Rivers region of northern Australia. Batch leaching tests on Ranger, Nabarlek, Koongarra and Jabiluka ores showed that uranium extraction was unaffected by choice of oxidant, but that Caro's acid reduced acid requirements by 15 - 25%. Lime requirements for neutralization of tailings liquors were reduced by 20 - 30%.The batch studies were extended to a four-stage continuous leaching circuit with a capacity of 400 gore h-I. Comparative leaching tests confirmed the reagent savings obtained in the batch tests. Following these encouraging laboratory results, lnterox Chemicals Pty Ltd carried out plant trials using Caro's acid. Reagent savings in the mill were similar to, or better than, those obtained in laboratory test work. The trials also established that Caro's acid has a number of operational advantages over pyrolusite.IntroductionUranium is most commonly extracted from its ores by leaching in sulphuric acid. Simple hexavalent uranium oxides and compounds are readily soluble but uranium in the tetravalent form is insoluble and must be oxidized for dissolution to occur. The most commonly used oxidants have been sodium chlorate and manganese dioxide. They act indirectly by maintaining iron as the ferric ion which oxidizes uranium by a surface electro- chemical reaction. An Fe3+ concentration of about 1 - 2 g L-I is usually considered adequate for the effective dissolution of uraninite(1)."

Jan 1, 1984

By A. J. Kwitowski

Remote control for mining machines ordinarily means the operator is not seated on the machine, but is located within direct view of the machine and work area Thus, remote control operators are exposed to the hazards of roof/rib falls and dust/methane explosions. The U.S. Bureau of Mines has developed a method to disassociate remote operators from these hazards. Off-board, computer-based "tele-operational" systems are utilized that station the operators one-hundred meters or more distant from the working faces. Details are provided for tele-operated systems for thin-seam extraction and haulage equipment in highwall and deep, room-and-pillar coal mines.

Jan 1, 1992

By Joe Komadina

DOUG HALBE: Our next topic is one that I would think everyone might want to contribute to. I'm sure everyone here has had some experience in this area. If you haven't, I'd suspect you've never really run a mill. This is what we call "Horrible Spill Areas We Had When We Started Up the Plant and How We Fixed Them." Our next speaker has had a really great operating career. He had many years with Newmont in the Carlin area, and now he's executive vice president and chief operating officer of Independence Mining Company: Jim Komadina. I don't have to be nice to the speakers anymore, do I? [laughter] You may wonder why we picked Jim Komadina to give this talk. I was involved many years ago in the start-up of Newmont7s Gold Quarry plant. Jim held quite a responsible position there. I'm not going to say anymore, but I have in the back of my mind this picture of the pump floor and a rowboat and a guy rowing around on the pump floor. [laughter] Jim, was that you? [laughter] JIM KOMADINA: Probably. I wasn't responsible for the design. [laughter] Actually it's amazing. I've seen a lot of these plants and actually had the opportunity to walk around them, so when I say this, "Horrible spills I have seen and done," it's because I've been responsible for more than my fair share of them. But having seen a lot of spills, I will present a little bit of wisdom about how to prevent them.

Jan 1, 1998

By R. K. Steinhorst

Multivariate cluster analysis, MANOVA, canonical analysis, and discriminant analysis of hydrochemistry data were used to investigate the directions of ground water movement in basalts in the vicinity of the Hanford Reservation, Washington. The statistical analyses indicate that the hydrochemistry of the ground waters in these basalt formations is distinctly different on each side of the Columbia River. This suggests that the river is a ground water divide or that the river is roughly coincident with a hydrogeologic barrier boundary. The statistical procedures used in this study constitute a quantitative means for differentiating ground waters according to hydrochemistry.

Jan 1, 1990

By J. Alfred Berger, O. M. Katz

Selected samples of hydrided Zr-Hf alloys were rapidly quenched to voom temperature and exrtrnined metallographically, by X-ray diffraction, and through micro hardness studies to confirm high-temperutuve data Confirming experiments sllowed that there were five phases in this Lernary system: 1) hextrgonal with lattice parameters similar to that of the initia1 Zr-Hf alloy but slightly enlarged due to dissolved hydrogen; 2) fee with properties of a brittle, intermediate, hydride compound; 3) fct with c/a crvoltnd 1.07 and which appeared as a neetilelike precipitale; 4) hexagonal, designated ?, with c/a ratio of 2.37; and 5) orthorhombic, designated X, with a = 4.67, b = 4.49, and c = 5.093 and whose tnicro-st?ruct~ival nppetrl-nnce depcncled o/i, heat lvecrt~r~ent. The tetragonrrl phase never crppeal-erl witkorct the cubic hydricle. Abpecrrtrnce of 0 and A also tlependet on the hafnium content of the zirconium. A previous paper' on the Zr-Hf-H system described the thermochemical data obtained with a high-vacuum, high-sensitivity mirrogravimetric apparatus. This data presented a fairly complete picture of the phase relationships at elevated temperatures. However, it could not establish the actual crystal structures, lattice parameters, or metallographic disposition of the hydride phases. The present complementary study utilizes X-ray powder patterns along with light and electron microscopy to characterize completely the five hydrided phases found in Zr-Hf-H alloys quenched to room temperature. Crystallographic features of the zr-Hf,2,4 zr-H,5-7 and Hf-H8 systems have been summarized in Table I. Designations of a, ß, and ? were retained in the Zr-Hf-H system for the phase regions through which the pressure-composition isotherms always sloped. However, it was not firmly agreed that these were single-phase regions.' In fact, the region designated y always contained a cubic as well as a tetragonal phase after quenching to -196°C. MATERIALS Preparation of the high-purity Zr-Hf alloys has been described.' The four zirconium alloys which were hydrided contained 37 wt pct Hf (23 at. pct), 51 wt pct Hf (37 at. pct), 73 wt pct Hf (58 at. pct), and 91 wt pct Hf (82 at. pct), respectively. These were designated B-2, B-4, B-6, and B-8. Photomicrographs of the initial alloys showed the material to be quite clean as would be expected from the precautions exercised in producing them. However, there were a number of annealing twins but no other subgrain structure. In addition to the four original alloys, fifteen hydrided samples were observed at room temperature. Hydrogen compositions are given at the top of Tables I1 to V. APPARATUS The phases present at elevated temperatures were studied by quenching hydrided samples to room temperature by two different methods, both under vacuum: 1) fast cooling of the sample tubes of the microgravimetric apparatus1'9 with flowing air and 2) rapid quenching into liquid nitrogen. The cooling rate for 1) was 750° to 250°C in 30 sec. Since the microbalance chamber was not designed to permit very rapid cooling of a hydride sample, all liquid-nitrogen quenching was done in an auxiliary experiment. The auxiliary quenching apparatus consisted of a small-bore, high-temperature furnace, a sealed SiO2 tube containing the sample, and a dewar quenching flask filled with liquid nitrogen. The hydrided sample, previously quenched in the microgravimetric reaction chamber, was placed in a platinum boat in a vacuum-degassed SiO2 tube. A zirconium wire getter and degassed SiO2 rod, to reduce the internal volume, were also in the tube. After sealing the tube under vacuum the zirconium getter was heated to absorb the last traces of gas. Only the sample was heated at the reaction temperature for the desired length of time, and then the tube dropped through the opposite end of the furnace into the dewar. A quenching rate of 200" to 400° C per sec was estimated. Analyses of samples after the auxiliary experiment also showed practically no increase in oxygen or nitrogen content from heating in the SiO2 tube. All of the samples were examined at room temperature by the X-ray powder method. The majority of the powder patterns were obtained with double nickel-filtered CuKa radiation after 8- and 16-hr exposures in an 11.48-cm-diam camera. Cobalt and chromium radiation were also used to spread out the high d value end of the Pattern. Such patterns readily identified the minor phases. NO oxide or nitride lines were found. Where sharp back-reflection lines existed it was possible to reduce the

Jan 1, 1965