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Jan 1, 1945

By E. J. Gleim

Contact with trolley wire in the mines of the United States has taken a considerable toll of life throughout the years that trolley locomotives have been employed as a means of' transportation. A study3/ of the records over a 15-year period for one State alone showed that, of 98 fatalities resulting from contacts with electrical circuits and equipment, 75 were caused by direct or indirect contact with unguarded trolley wire in coal mines. The law relating to guarding trolley wires in the mines of this particular State, as amended in 1935, reads in part as follows: "All trolley wires carrying 220 volts or more, and less than six feet six inches above top of rail, must be guarded at all points under which men and animals are required to pass***,'" The natural conclusion to be drawn from such records is that lack' of guards or shields must be held responsible for these fatalities. As a preventive measure, it has been advocated that every foot of trolley wire in mines should be guarded. Although some such drastic steps may appear to be amply justified, closer examination of the records nor this and other coal-mining States shows that absence of guards is not entirely responsible; but rather that other factors, such as carelessness and neglect it the observance of certain well-established simple rules concerning installation and location of trolley wires, also are responsible. In other words, if trolley wire is installed carelessly and its maintenance is neglected, it should not be expected that the mere installation of guards will overcome such carelessness and neglect. This publication discusses Various types of guards that have been used in Coal and metal mines of this country, together with related steps bearing upon the problem of 'preventing shock and fatalities from contacts with trolley wire. The material herein contained is taken largely from Information Circular 6577,4/ now out of print, and has been revised to include some types of guards that have been used in metal mines, together with a discussion of guard materials not covered in that publication.

Jan 1, 1945

By J. A. Reid

THE views and observations expressed herein on this old but constantly recurring question are our own, no effort having been made to align them with standard texts. Therefore, while they may find general acceptance amongst fellow engineers, they must stand as personal opinions and as such are open to debate and discussion. In order properly to consider the subject, it should first be 'set in proper perspective. Why are Prospects Examined? Prospects are examined to determine whether they may contain economic concentrations of metals or minerals, the legitimate mining business being run, pretty largely, to make money. Next to food and clothing, modern civilization is based on metals, with which are included in this discussion minerals, oils, and fuels. A constant and increasing demand for the common metals requires the location of replacements for depleted orebodies, while the use and appreciation of new metals brings increasing demand for them. Aluminium is a good example of a metal which has, within recent years, made great progress. Today, we are becoming increasingly aware of magnesium, chromium, tungsten, thallium, and other lesser known, metals.

Jan 1, 1945

By E. C. Roper

THE Britannia Mining & Smelting Company, Limited, have been operating their property at Britannia Beach, B.C., continuously for nearly forty years and have mined over 33,000,000 tons of ore from orebodies within a belt of highly sheared rocks, five miles long by 2,000 feet wide. The property is in the Coast Range mountains, about twenty miles due north of Vancouver. The mountains rise abruptly from sea level to elevations of 4, 500 feet within a horizontal distance of 7,000 feet. The topography has enabled the orebodies to be developed by adit tunnels. The active mining levels are connected to the adits by incline and vertical service shafts. The main service adits are the 2200, 2700, and 4100 levels (see Figure 1). The mine surface shops, three bunk-houses, and over one hundred dwellings form the townsite camp at the portal of the 2200 level adit. A small camp of one bunk-house and a few dwellings is situated at the 2700 level portal. The beach surface shops and camp, adjacent to the 4100 level adit, service the mill, foundry, and other beach installations as well as the mining from the 4100 level. The ore mined from the various orebodies is delivered to the 4100 main haulage level through a system of rock raises and intermediate tramming levels and is hauled on the 4100 level to the mill.

Jan 1, 1945

By R. D. Leitch

From time to time the Bureau of Mines has received requests from persons who wish to destroy unwanted explosives, and although the information that follows has been accumulated from sources considered reliable,4/ the. Bureau of Mines assumes no responsibility for accidents that may result from following the suggestions offered. Explosives to be destroyed may be fresh material from damaged packages, usable material for which there is no further need, or material that has deteriorated either from natural aging or from improper storage to the point where it is unfit for use.

Jan 1, 1945

Jan 1, 1945

By W. R. Toeplitz

H. N. Ghenn.*—It has been established that the accuracy obtainable from any precision machine is a function of the wear resistance, maintenance and closeness of fit of the bearings, hence I would like to ask Mr. Toeplitz how these oil-less bearings compare with cast iron or babbitt or similar materials when used on precision machinery. Could these bearings be used, for example, on a grinding machine in which work must be held to a tolerance of plus or minus 0.000025 inch? W. R. TOEPLITZ.—The metal-powder bearings can be held to very close tolerances and are used in place of cast iron and babbitt on precision machinery.

Jan 1, 1945

By G. M. Furnival

A PROGRAMME of structure drilling was commenced in the Southern Alberta Plains in June, 1943, for the purpose of determining the geological structure of the underlying sediments. More than 270 holes have been drilled throughout an area of some 1,800 square miles or 1,000,000 acres (see Figure 1). The Southern Plains of Alberta are covered by a mantle of glacial drift,' at places exceeding 200 feet in thickness. Only where this mantle has been dissected by deep drainage channels is bed-rock exposed to any great extent. Along such channels, surface geological mapping can be conducted to ad- vantage. Accordingly, geological mapping was commenced _in 1942 and continued each season to the present. To supplement this information, a survey of the water wells was carried on in conjunction with the mapping. However, to obtain more positive and evenly distributed structural control throughout the area as a whole and to define more adequately structural trends indicated by the preliminary mapping, it was necessary to resort to the use of drills to penetrate the glacial mantle. Various types of light drills are commonly used for this purpose and provide geological information in the form of drill cuttings, cores, drilling time rates, etc. Correlation of information is generally obtained through comparison of cored sections, drill cuttings, micro-fossils, and drilling time rates. However, in this case the holes were electrologged and correlations were made chiefly by comparison of such logs. The data so obtained is plotted and portrayed in the form of structure contour maps on recognizable stratigraphic horizons and in the form of isopach maps of the recognizable stratigraphic intervals penetrated in the holes. This method had not been widely used in Alberta previously and the technique employed was necessarily developed after the project began.

Jan 1, 1945

By Carl F. Floe, Michael B. Bever

THE possibility that carbon may be soluble in copper to a limited extent has been recognized for over a century. The quantitative investigation of this problem, however, requires more sensitive techniques than have formerly been available. Three recent developments have made possible more accurate determinations: the vacuum-fusion method of analysis, the production of copper of high purity and the availability of high-purity refractories, particularly graphite. In addition to its obvious theoretical interest, the problem of carbon solubility in copper is of practical importance. In the production of copper and of high-copper alloys, carbonaceous covers are frequently used. If even minute amounts of carbon are dissolved, insoluble carbon oxide gases will be formed when such metals are poured under oxidizing conditions. A mechanism of this kind could well be one of the principal causes of gas porosity in casting copper-base products. REVIEW OF LITERATURE In 1823 Vivian1 raised the question as to whether copper by overpoling becomes "combined with a minute portion of carbon." Karsten2 asserted, in 1832, that carbon reduces the high-temperature strength of pure copper, so that when the carbon content has reached 0.2 per cent the metal will be brittle at a dark red heat. According to Karsten, carbon contents of o.05 per cent make it difficult to hot-work copper. He also reported that the specific gravity of copper is 8.8969 and that it increases to 8.92 58 if the copper is cemented with carbon and then melted. He emphasized the difficulty of determining analytically the small amounts of carbon present in copper. The metal was removed by wet methods and the residue considered as carbon. At Percy's request, Dick,3 in 1856, carried out various working tests on copper that had been in prolonged contact with carbon, and found that the working properties of the metal had not been affected. He also attempted to determine the presence of carbon analytically. In one experiment the copper was dissolved and the residue was fused with litharge, and in another essentially a combustion analysis was made on a copper sample. In a final experiment, a sample was dissolved and the residue subsequently subjected to a combustion analysis. Indications of as much as o.005 per cent carbon were found, but Dick considered his work inconclusive largely because of the possible interference of sulphur. Percy4 concluded, from Dick's experiments and from some experimental work of his own, that the solubility of carbon in copper had not been established with

Jan 1, 1945

By D. V. Carter, Dan C. Williams, John R. Coombs

Exploration was active in East and East Central Texas during 1944. Ten oil fields were discovered during the year, of which four show promise of development. The discovery wells of the Sand Flat and Tyler, South fields were drilled to a depth greater than 10,000 ft., and the latter field now produces from the Pettit at a depth of 9890 ft. The Sand Flat well was plugged back to the Paluxy. The other two fields are Glen Rose producers near 8000 ft. The Pickton field produces from the Bacon Lime and Winnsboro from the Rodessa section. The Eylau field, Bowie County, was significant as the first Smackover production in Texas. Magnolia drilled a test in the Concord field, which topped salt. The most extensive and significant development in the district was the Carthage gas-condensate field. It expanded from the 8000 acres of last year to an estimated 190,000 acres, or about 300 sq. miles, and is not defined as yet. The first oil production in the Carthage area was made from the Travis Peak in 1944 in the Rogers Lacy's Cameron Lumber Company well No. I, on the northwestern side of the field. The New Hope field, Franklin County, scored the largest number of completions during 1944 with 24, bringing its total number of wells to 27. Two more pays were opened and produced as dual completions with the older horizons. The Manziel field, Wood County, had 19 new wells added during the year, for a total of 29, while the Pittsburgh field, Camp County, reached a total of 23 wells by completing 14 new ones. Material shortages and drilling restrictions dropped the total number of producing wells completed in the district from 171 during 1943 to 141 for 1944. Abandonments increased from 531 during 1943 to 609 for 1944. Of this number, 479 were in the East Texas field. Subsidy payments had very little effect in the district and it was mostly a few of the old fault-line fields that had any wells to fall within the requirements for subsidy payments. The prices of crude oil remained constant in the district except for increases as a result of subsidy payments. Production and Probation Wartime demands called for increased allowables for many fields, consequently the condensate and oil production for 1944 increased to 190,016,180, which is up 6.9 per cent over 1943. The East Texas field, of course, remained the principal producer of the district, accounting for 134,768'499 bbl. during the year, or 71 per cent of the district total production of condensate and oil. The field topped its own 1943 production by 4.8 per cent and became the first field in the world to produce 2 billion barrels of oil. The Hawkins field remained the second largest oil producer in the district, with 13,317,088 bbl. for the year, a drop of 6.8 per cent from 1943, while Van field was third with 11,635,708 bbl. The

Jan 1, 1945

By N. Tiner

In an article on magnesium and its alloys, Gann and Winston! stated that manganese has a limited solubility in the liquid state. W. Schmidt2 showed a diagram according to Joseph Ruhrmann indicating that the solubility of manganese in liquid magnesium falls from about 2.65 per cent at 790°C. to about 0.5 per cent at 675°C. The curve was extrapolated to show zero solubility at the melting point of pure magnesium (Fig. I). This work suggested that at the lowest manganese contents it was not possible to detect either a eutectic or the formation of a solid solution, so that manganese was stated to be present in the structure as large individual crystals. Two years after the presentation of, these results, Gann3 brought evidence to show that some manganese is capable of dissolving to form a solid solution, any excess of manganese present then assuming chiefly the form of small blue-gray particles scattered throughout the primary magnesium crystals, occasionally in clusters but seldom at the boundaries. He presented micrographs of cast alloys containing 0.1, 0.4 and 1.0 per cent manganese that show a small amount of coring around the individual particles due to solid solution, and indicate that the location of the manganese particles is closely associated with the original dendritic structure of the primary crystallization. He also pointed out that the amount of manganese that can be dissolved in magnesium depends on the amount of other alloying elements present, the effect of the second alloying element being to decrease the amount of manganese retained in the alloy. E. Schmid and G. Siebe14 have determined the solid solubility of manganese and its variation with temperature by means of precision X-ray diffraction measurements. They found that the solubility is 3.4 per cent at 645°C. and decreases to practically zero at 200°C. It is apparent that the X-ray diffraction measurements of Schmid and Siebel are not in agreement with the results of Ruhrmann as presented by Schmidt. This disagreement, and also the lack of data on magnesium-aluminum-manganese and magnesium-zinc-manganese systems, led the author to the present investigation, to determine accurately the liquid solubility of manganese and its variation with temperature. Experimental Method The experimental method for making solubility determinations consists of saturating the molten magnesium or the alloys with manganese at various temperatures and analyzing the dip samples taken from these melts. Melting is carried out in a cylindrical steel pot heated by an electric resistance furnace. The pot had a metallic outside coating to protect the steel against oxidation, and a graphite inside lining to prevent the contamination of the melt by prolonged contact with iron. The inside diameter of the pot was 4 in. and the depth 12 inches.

Jan 1, 1945

By F. R. Hensel

PURE silver and silver-lead alloys have been studied as to their suitability for bearings.1-8 A review of the properties of thallium and the silver-thallium constitutional diagram was made by the author to analyze the possibilities of silver-thallium compositions for antifriction materials.† The silver-rich end of the diagram as reported in the literature9-11 was found to be sketchy and it was necessary to carry out considerable experimental work to arrive at definite conclusions. Some of the results of this work are reported in this paper. TEST MATERIALS In the beginning of the work, only fused alloys were investigated. Later, research [TABLE I. Composition of Fused Silver thallium Alloys Tested for Antifriction Properties PERCENTAGE ALLOY No.OF THALLIUM 15330.48 153406 231 HT2.04 2312.10 232 HT3.83Balance 2324.07Silver 233 HT5.86 2336.38 2349.84 234 HT10.07] was carried out on electroplating methods and diffusion processes. In preparing the fused alloys, care was taken to exhaust the toxic fumes caused by the thallium content. The compositions of the series of fused alloys are listed in Table I. The silver-thallium alloys were melted in clay-graphite crucibles and cast into preheated steel molds of 3/4-in. diameter. In the cast condition, they showed a cored structure, as indicated by the micrographs of Figs. I to 3. The etching reagent used was a mixture of 2 grams K2Cr2O7, 8 c.c. H2SO4, and 100 c.c. H2O. The cored structure is unsatisfactory for the type of corrosion resistance required for bearing applications, and homogenizing experiments were carried out at various temperatures, the results of which are shown in Figs. 4 through 8. The alloys with a lower thallium concentration, which were heated for 2 hr. at 525°C. show an almost completely homogenized solid solution type of structure. With higher thallium concentration, the homogenizing temperature was dropped to 475°C. to eliminate the formation of a liquid phase. It is evident that heating for 2 hr. at this temperature did not result in complete elimination of the cored structure. As would be expected, cold-working of the cast structure is an expedient in establishing equilibrium conditions. The fine homogeneous grain structure shown in Fig. 7 corresponds to the cold-worked area under the Rockwell ball penetration when the hardness was taken before heat-treatment. A detailed structural study was made on a cast silver-thallium alloy containing 3.67 per cent thallium. Three micrographs (Figs. 9, 10 and 11) show the transition

Jan 1, 1945

By C. G. Kemsley

THE ore as hoisted is very wet, and difficulty was experienced i~ screening it to remove the fines before going to the secondary crusher. In fact, the fines had a tendency to form balls and roll down the screen, and only a small percentage was removed. Their inclusion with the other ore going to the Symons secondary crusher caused excessive spring action and pounding between the adjustment ring and main frame, resulting in abnormal wear between the two. To overcome this, it was decided to wash the fines through the primary screen, and use an Akins classifier to de-water the screenings, pumping the overflow from the classifier up to the mill and discharging the oversize onto the mill-feed belt.

Jan 1, 1945

By Claus G. Goetzel

PRESSING of powdered metal parts is best done in the direction of the shortest extension of the piece, to avoid too great a loss of pressing force through internal [ ] friction. As long as curved surfaces, recesses, or offsets occur only parallel to this shortest axis of pressure, no special difficulties arise: the cross sections, perpendicular to the pressure, do not vary, nor does the shape of the parts change during compression except for a gradually reduced thickness (Fig. IA). The problem becomes more difficult, however, when the curved surfaces or recesses are perpendicular to the shortest axis of the part (Fig. IB). Two processes for molding uniformly dense parts with complicated shapes from powdered metals are described in detail in this paper. Both can be employed successfully by those trained in the art. The first refers to curved parts; the second is especially adapted to parts having one or more recesses or steps. Both methods, as set forth here, are applied under the condition that presents the more difficult problem. For clarity, before description of the two practical methods, the variable factors in molding powdered metal parts will be reviewed, then an idealized procedure will be considered briefly. VARIABLE FACTORS IN MOLDING POWDERED METAL PARTS Compression Ratio Compression ratio is defined as the proportion of the final relative density of the compact to the apparent density of the powder. For iron powder of an apparent density of 3.0, for example, a compression ratio of 2 1/2 : I would be required to produce a compressed compact of 7.5 density; whereas for another iron powder having an apparent density of only I.5, a compression ratio of 5:I would be required to produce the same density. The lower the powder's apparent density, the greater must be the compression ratio for pressing compacts of high density.

Jan 1, 1945

By D. C. Porterfield

ProUuction of crude oil in Venezuela increased from 186,134,000 bbl. in 1940 to 2~8,131,ooo bbl. in 1941, or 22.6 per cent, to establish a new all-time high for the country. While the average production for the year was 625,000 bbl. per day, production during the month of December 1941 averaged 751,000 bbl. per day, and during the last week of the year, 766,000 bbl. per day. Production from the Lake Maracaibo basin averaged 454,000 bbl. per day during the year, or 72 per cent of the total for the country, compared with 73 per cent of the total produced in 1940. Drilling during the year was approximately on the same scale as in 1940, with 438 wells completed in 1941 as compared with 429 the year before. Exploratory completions decreased from 18 in 1940 to 6 in 1941. Of the drilling operations in 1941, 56 per cent was concentrated in the Lake Maracaibo basin and 44 per cent in eastern Venezuela, success being 98 per cent in the Lake basin and 83 per cent in the east. Successful completions for the country as a whole amounted to 92 per cent of the total wells drilled. Exploratory drilling in 1941 resulted in the discovery of three new fields, all in eastern Venezuela; viz., Guara, about II km. to the northeast of the Oficina field but on a separate structure; Santa Rosa, which is east of El Roble field on a structure forming a part of the major Santa -Ana- San Joaquin-El Roble uplift; and Santa Barbara, which is southwest of the Jusepin field on an extension of the main Jusepin anticline. At the close of the year three wildcats were drilling, all of which showed prospects of obtaining production; that is, Mercedes No, 2 in central Guarico, Las Ollas No. I on the Anzoategui-Guarico border near the town of Zaraza, and Quiamare No. I in Anzoategui northeast of the town of San Mateo. In spite of heavy withdrawals and the resultant natural decline in the potentials of older producing areas, new drilling during the year increased the potential production of the country from an estimated 780,000 bbl. per day at the end of 1940 to an estimated 810,000 bbl. per day at the end of 1941, or approximately 4 per cent. Since domestic consumption of petroleum products is insignificant compared with total production, exports of crude and products during the year increased in line with production. Crude exports totaled 196,800,000 bbl., compared with 158,400,-000 bbl. in 1940, and exports of products were 26,100,000 bbl., compared with 21,900,000 bbl. the year before. Exports of crude from Venezuela to the United States amounted to 36,500,000 bbl. In addition, about 2,200,000 bbl. was imported in bond into the United States for transfer to Canada. Total refining capacity of the country in 1941 was approximately 125,000 bbl. per day, including a crude-conversion plant with a capacity of 32,000 bbl. per day, capable of making fuel oil only. Three plants with a capacity of 121,000 bbl. Per

Jan 1, 1945

By T. V. Lord

Minerals containing uranium have been successfully pre-concentrated by flotation at Queen's University, Kingston. In particular, uraninite, uranothorite, euxenite, and fergusonite, have responded to flotation to yield grades of 0.2 to 6.0 .per cent U .o. with recoveries of 85 to 98 per cent, from heads analysing approximately 0.10 per cent U3Os. Of the ten or so radioactive samples examined to date, two distinct groups were recognizable, firstly, those samples in which uranium was the sole constituent of economic interest, and, secondly, those in which Columbium (with minor amount of tantalum) was present in addition to uranium. For the purpose of this paper, the results of investigation on two samples of each of the above groups have been selected as typical.

Jan 1, 1945

The Joint Session on Continuous Cast- ing, of the Institute of Metals Division and the Iron and Steel Division of the American Institute of Mining and Metallurgical Engineers, convened in the Jade Room of, the Hotel Waldorf-Astoria, New York City, on Feb. 23, 1944, at 9:15 o'clock, Carl E. Swartz presiding. C. E. SWARTZ.-It is gratifying to see so many out at what may seem an early hour for the beginning of A.I.M.E. sessions, but I think this number-some fifty or sixty of you-is an adequate expression of the interest in these processes all over the United States, and possibly in foreign countries. I would like to ask those who feel that this type of program is of value to you to write or speak to some one of the Institute of Metals Division officers and suggest other topics for symposiums. We have a feeling that some of these current practices are of interest and we believe that under proper sponsorship many of the companies will be willing to give publicity to processes such as those that will be discussed today. Also, we would like suggestions and criticisms, so that the next ones can be better. The subject of continuous casting is not new, of course. The two papers on the program this morning will adequately cover the history and some of the earlier processes, some of the theory and some of the practice, some of the reasons why these various methods did not work. I was rather interested in discovering, when thumbing through one of the A.I.M.E. publications the other night, an article on continuous casting. I was not aware that the A.I.M.E. had published any papers on continuous casting, but there may be a number. The one that I happened to find was published in the 1915 volume, on the Mellen rod- casting process, and so we might say this is not the first session in which these subjects have been under discussion. However, there have been many improvements since then in all fields of metallurgical and mechanical engineering; consequently, I think that the papers today will be a little more involved and a little more complete in their technique. The first paper today will be given by one of our gentlemen of the press, who has done one of the outstanding jobs in this country in calling to our attention some of the newer processes that are being considered and being used in the metallurgical indus-

Jan 1, 1945

By C. G. Dunn

Identification of the kinds of orientation relationships that may exist among crystals is an important problem in the metallurgical field. As an aid to its solution standard orientations of several orders of twins would be very useful for rapid analyses to discover high-order as well as low-order twin relationships. Although data have been published that give orientations for three generations of twins, these data are not readily useful in the form presented; i.e., in a stereo-graphic projection with one pole per orientation.' However, accurate data based on calculations of the positions of all {1001 planes for such groups would be very useful when presented in tabular form. Therefore, calculations have been made for a group of four orders of twins and the data are listed in Table 3. Illustrative applications are considered briefly, with the idea of pointing out what may be done with large groups of orientations. Method of Computing Orientation OF a Twin It is common practice to describe the orientation of a crystal in terms of the positions on a stereographic net of the poles of certain planes of the crystal. A single position on a net may be given in terms of two angle variables, two sets of which appear in the following equations: Polar Net Wulff Net x = , sin ?p cos Fbp x = r COS ?w y = r sin ?p sin Fp y = r sin ?w cos Fw % = r cos ?p z = r sin ?w, sin +, The three numbers z, y and z determine a length r as well as a direction (0, 4) in an X, Y, Z coordinate system. In the present case, r will be set equal to (h2 + k2 + L2)1/2, where h, k and I are the usual Miller indices for a crystallographic plane, a restriction that facilitates determination of the positions of poles of new planes from those of old or known ones,2 as will become evident later. Furthermore, since twinned lattices have certain planes in common, it is an easy matter to determine the orientation of a twin of a crystal if the orientation of the crystal itself is known. We start therefore with a crystal of known orientation (positions of three {Ioo} poles given) and determine where the cube poles occur in first, second, third and fourth-order twins. Methods for identifying twinned lattices and for making the calculations to find the orientation of a twin have been published.3,4' Reference 4 will be illustrated in the calculation of the orientation of a twin, even though this method differs from the one used by the writer in obtaining the following data on four orders of twins. Consider a crystal S and its twin A1, A' being one of the four {112} or {III} type* first-order twills of S. The orientation of S—i.e., the positions of poles of (I00)

Jan 1, 1945

By A. B. Hooker

A list of permissible mine equipment, tested and approved by the Bureau r. Mines previous to January l, i-)4, , was published in Bureau c Moines In ornation Circular 7207.3/ The l ,.t c -. that dote was complete as to equipmentthen available and in current Information Circular 7210,?+/ published as a supplement thereto, listed equipment approved during; the calendar 1942. Information Circular72x'3,_/ published as a second supplement thereto, ! listed equipment approved during the calendar year 1943. The present listis. Another supplement covering approvals issued during the calendar year 1c)44. The items are numbered crud to indicate the consecutive order in which each typo of machine or device was approved _.c?. in its particular classification. Thus Information Circular 7207 gave 1,t drills and drilling much fines on the Bureau'sactive.. d active list Ih: additional anal approval: were given in 1942 the three issued in 19 and one issued :n 1944- bring the total to `3. Item 111, under. Loading Machines and conveying appeared in lnformation Circular 7207. It is repeated ',tore to _how that on j,,l was granted Curia 1the optional of this loader when modified .'or 2 0. alt ciruits .]

Jan 1, 1945

By George A. Moore

A recent survey of existing analytical results, and an attempt to correlate them with each other and with the known history and behavior of the samples, indicated that none of the commonly applied methods could be considered established as intrinsically reliable. It was. therefore, desired to attempt to establish the reliahility of some one method by external evidence. If this were to be accomplished, other methods could then be evaluated in terms of the method establibhed. The correct method was accordingly to be chosen without regard for cost, speed, or convenience; with the requirements for routine application to be reserved for 1ater consideration. The method of total combustion was chosen and submitted to a limited number of tests against primary standard samples. Considerable experimental difficulty was encountered, indicating that additional work on the experimental arrangements is desirable. While the work to (late by no means represents a completed investigation, it is helieved that the combustion method is basically sound and that its development should be continued. Choice of Method Of the several available methods, mechanical disintegration. electrochemical methods'2'3 modifications of the Sieverts experiment,% and vacuum fusion, were all judged to contain one or more factors of un- certainty not at present completely cvaluated or suhject to complete control. These methods, therefore, were considered currently unsuitable for referee purposes. Solid evolution was considered to be of doubtful significance when conducted in the alpha range. A reasonable chance for a true analysis was found for evolution in the gamma range. Preliminary tests have indicated a very slow rate for evolutioll from gamma iron. indicating a running time of possibly 100 hr. for a one-centimeter sample. Difliculty in distinguishing such slow. evolution from blank gas was anticipated, hence the method was not consitlerctl the most suitable for the present purpose. The combustion method was evaluated as being most sound on fundamental principles. The only important unknown would be to determine that the iron oxide formed did not occlude water at the tcmperaturv of the combustion.with the odvious precautions of using a sound and clean specimen, providing a system sufficiently tight to give acceptable blanks in longtime runs, and providing a suficicntly sensitive measuring system, reasonable, precise, and truthful analytical results could be logically expected. Apparatus The equipment as originally operated is shown in Fig. I, and the glassw-are in its latest modification in Fig. 2. The sulphuric acid drier and small safety tube in the upper right of Fig. I were replaced by a KOH drier and combined manometer safety tube, to permit operation at reduced

Jan 1, 1945