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By F. Louis Grammer

THE difference between blast-furnace gas and ordinary producer-gas is chiefly that blast-furnace gas is richer in CO, and poorer in hydrocarbons and hydrogen, as is shown in Table I. TABLE I.-Volume-Composition of Producer-Gas and Blast-Furnace Gas.. Producer-Gas. Blast-Furnace Gas. Per Cent. Per Cent. (Volume.) (Volume.) CO . 22 to 33 25.5 00., . 6 to 3 13.0 H . . 13 to 7 1.5 CH, 3 to 1.5 0.0 N . 54 to 60 60.0 If natural gas, water-gas, or by-product coke-oven gas be available, blast-furnace gas can be made to resemble very closely in calorific value the average producer-gas by merely mixing in one of these products, which are richer in hydro-carbons and, hydrogen. Blast-furnace gas, however, possesses a virtue which is sometimes absent in producer-gas, especially with coals very high in sulphur-namely, that blast-furnace gas is relatively free from sulphur. In some regions the sulphur in coal is an acute problem, and it is highly desirable to find uses for the products which are specially high in sulphur-content. An advantage would be gained if coal was coked before charging into the gas-producers, but this adds to the expense. Sulphur may be partly eliminated from coal by washing it, the success depending upon the form in which the sulphur occurs, and upon the efficiency of the washer, but it cannot always be removed to the extent desired at most American plants. It is not practicable to remove all the sulphur from producer-gas by washing it, though Mr. Reinhardt, of Germany,

Sep 1, 1908

By AIME AIME

ON March 14, the University of Tulsa was accepted as a member of the North Central Association of Colleges, which ranks Tulsa among the leading universities of the country. A. G. OIiphant recently donated to the new school of petroleum engineering a splendid collection of books on geology, valued at $25,000. Waite Phillips, an oil producer and chairman of directors of The Independent Oil & Gas Co., donated $150,000 for a petroleum engineering building

Jan 1, 1929

Mr. John J. Porter, Chicago Ill. (communication to the Secretary†):—Mr. Baker's account of his experiences with stock-distribution has been particularly interesting to me, as it

Jan 1, 1905

By William E. Ford, Edward Salisbury Dana

1. Normal Class (6) Zircon Type 2. Hemimorphic Class (7) Iodusuccinimide Type 3. Pyramidal Class (8) Scheelite Type 4. Pyramidal- Hemimorphic Class (9) Wulfenite Type 5. Sphenoidal Class (10) Chalcopyrite Type 6. Trapezohedral Class (11) Nickel Sulphate Type 7. Tetartohedral Class (12) Mathematical Relations to the Tetragonal System THE TETRAGONAL SYSTEM includes all the forms which are referred to three axes at right angles to each other of which the two horizontal axes are equal to each other in length and interchangeable and the third, the vertical axis, is either shorter or longer. The horizontal axes are designated by the letter a; the vertical axis by c (see Fig. 166). The length of the vertical axis expresses properly the axial ratio of a : c, a being uniformly taken as equal to unity. The axes are orientated and their opposite ends designated by plus and minus signs exactly as in the case of the Isometric System. Seven classes are embraced in this system. Of these the normal class is common and important among minerals; two others have several representatives, and another a single one only. It may be noted that in four of the classes the vertical axis is an axis of tetragonal symmetry; in the remaining three it is an axis of binary symmetry only.

Jan 1, 1922

By L. F. Mashburn, T. J. Ferree

A Reichert cone concentrator was installed in an aggregate plant circuit to recover the extremely fine "flour gold" known to exist in the deposit. The gold content of the bank- run gravels averages about 0.1 g/t-about $1.29/t, based upon $12.86/g ($400 per oz) gold. The fineness of the gold averages between 950 and 960. The Reichert cone, in conjunction with a conventional shaking table, recovers in excess of 85% of the gold. A screen analysis of the gold particles shows 44.1 % is - 74pm (-200 mesh) in size. The plant operates with a two-man crew.

Jan 1, 1983

By Michael B. Bever, Carl F. Floe

The solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to I300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. Review of Previous Work The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar5 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwasé3 reported large hydrogen solubility values for several compositions of copper-tin alloys, which appear to be in error.

Jan 1, 1944

By Carl F. Floe, Michael B. Bever

The solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to I300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. Review of Previous Work The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar5 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwasé3 reported large hydrogen solubility values for several compositions of copper-tin alloys, which appear to be in error.

Jan 1, 1944

I PRESIDING OFFICER At all business meetings of the Institute the President, or, in his absence, the First Vice-President, or, in the absence of both of them, any other Vice¬ President or Director, chosen by the meeting, shall preside At all other meetings of the Institute the President, or, in his absence, one of the Vice-presidents shall preside If none of these be present the meeting shall elect a Chairman The President shall do and perform such other duties as may from time to time be assigned to him by resolution of the Board of Directors of the Institute II ORDER OF BUSINESS At each business meeting of the Institute the order of business shall be as follows 1 Reading of minutes of preceding meeting 2 Report of the President 3 Report of the Treasurer 4 Report of the Secretary 5 Election of Directors 6 Reports of Standing Committees 7 Reports of Special Committees 8 Special Orders 9 Miscellaneous business This order of business may be changed at any meeting, by a vote of a majority of the Members and Associates present At all sessions of the Institute, other than business meetings, the order of proceedings and the time of adjournment shall rest in the discretion of the presiding officer

Jan 1, 1923

I. PRESIDING OFFICERS. At all Business meetings of the Institute the President, or, in his absence, the Vice-President, or, in the absence of both of them, any other member of the Board of Directors to be chosen by the meeting, shall preside. At all other meetings of the Institute the President of the Council or, in his absence, one of the Vice-Presidents, if present, shall preside II. ORDER OF BUSINESS. At each Business meeting of the Institute the order of business shall be as follows 1. Reading of minutes of preceding meeting. 2 Report of the President. 3. Report of the Treasurer. 4. Report of the Secretary. 5. Election of Directors. 6. Reports of Standing Committees. 7. Reports of Special Committees. 8. Special Orders 9. Miscellaneous business. This order of business may be changed by a vote of a majority of the Members and Associates present in person or by proxy. The usual parliamentary rules shall govern all meetings of the Institute except in cases otherwise provided by the Constitution or the By-Laws. At all sessions of the Institute other than business meetings, the order of proceedings and the time of adjournment, shall rest in the discretion of the presiding officer

Jan 1, 1923

By Sam Tour

OF the new alloys achieving commercial prominence during the year, an aluminum-silicon magnesium casting alloy, which is similar in many respects to the 4 per cent copper alloy, developed about 1921, which has attained such a wide field of service, may be mentioned. The new alloy, like the old, is a heat-treatable type and develops about the same physical properties. The alloy casts easily and is relatively insensitive to high pouring temperatures. Its ability to produce substantially leak- proof castings is noteworthy. A second casting alloy development is the new Aluminum Co. of America No. 132, "Lo-Ex" piston alloy, a result of nearly eight years of research. The alloy contains about 14 per cent silicon and varying amounts of nickel, copper, and magnesium. It exhibits a low coefficient of expansion and thus permits small piston clearances. Its lower specific gravity is a further advantage.

Jan 1, 1932

By AIME

Compiled by Mary Ann Gross, Department of Energy. Bruceton. PA. Supplemental data from Coal Age indicated by (*). Reprinted by permission from CoalAge magazine.

Jan 1, 1981

I. PRESIDING OFFICERS. At all Business meetings of the Institute the President, or, in his absence, the Vice-President, or, in the absence of both of them, any other member of the Board of Directors to be chosen by the meeting, shall preside. At all other meetings of the Institute the President of the Council or, in his absence, one of the Vice-Presidents, if present, shall preside II. ORDER OF BUSINESS. At each Business meeting of the Institute the order of business shall be as follows 1. Reading of minutes of preceding meeting. 2 Report of the President. 3. Report of the Treasurer. 4. Report of the Secretary. 5. Election of Directors. 6. Election of Members of the Council. 7. Reports of Standing Committees. 8. Reports of Special Committees. 9. Special Orders 10. Miscellaneous business. This order of business may be changed by a vote of a majority of the Members and Associates present in person or by proxy. The usual parliamentary rules shall govern all meetings of the Institute except in cases otherwise provided by the Constitution or the By-Laws. At all sessions of the Institute other than business meetings, the order of proceedings and the time of adjournment, shall rest in the discretion of the presiding officer

Jan 1, 1923

By H. M. Bannerman, E. N. Cameron

INTRODUCTION DURING the years 1942-1944, about 125 New England deposits were mined for sheet and punch mica, and many others were briefly prospected. During this period the Geological Survey, United States Department of the Interior, carried on detailed studies of the deposits and the pegmatite bodies that contain them. The primary purpose of the studies was to provide geological information that would contribute toward efficient mine development and operation. The studies were aimed directly at practical production problems. Detailed maps showing the structure of the deposits were prepared, and geological findings were closely correlated with data on specific yields and costs of mining and processing. The result is information that permits a reasonably accurate appraisal of the mica deposits of New England and the mining industry that they support. At a time when the future of the industry is in doubt, it seems desirable to submit this appraisal for consideration. Domestic mica deposits supply only a small fraction of the country's needs in normal times, for only the richest domestic deposits can compete with the low-cost mines of India and Brazil. However, the possibility that this country may be cut off from its supplies in time of war gives domestic deposits an importance much greater than their peacetime production would imply. New England supplied about 22 per cent of domestic output in 1943 and 1944, the peak years of wartime production. Its actual contribution to the war effort was greater, for the proportion of sheet mica of high quality in the New England product is higher than the average for domestic mica. The data analyzed below were collected for the Geological Survey by D. M. Larrabee, A. H. McNair, J. J. Page, V. E. Shainin, G. W. Stewart, and the co-authors of this paper. The cooperation of officials of Colonial Mica Corporation and of mine operators and owners in furnishing information is gratefully acknowledged. D. M. Larrabee, A. H. McNair, and V. E. Shainin have made various suggestions based on critical reading of the manuscript. ANALYSIS OF WARTIME OPERATIONS In considering the data presented in this report, it must be remembered that the scale of mica operations is very small compared with that of many other mining industries. The typical New England mica mine of 1943 and 1944 was worked by a crew of five or six men. Equipment was varied but on the whole extremely simple. The first stage of operation at a deposit was normally opencut mining. Drilling was done mostly with jackhammers powered by portable compressors driven by gasoline engines. Muck was shoveled by hand into buckets with a capacity of 1/3 to 2/3 ton and commonly hoisted by derrick to a dump adjacent to the cut. As operations were carried to greater depth, and the transition to underground mining was made, these methods were modified to a degree depending largely on the attitude of the deposit mined. At steeply dipping deposits,

Jan 1, 1946

By Charles Catlett

AN examination of the census reports' for 1880, which contain a large number of complete analyses of typical American iron-ores, indicates that the existence of barium sulphate in intimate association with iron-ore is rather unusual. Of 94 analyses reported there, but four show any barium sulphate, and the maximum content amounts to 3.04 per cent. The note of the occurrence of considerable quantities of barite in connection with certain iron-ores found in the Pinar del Rio Province of Cuba may be of interest. These deposits are found near the little village of Francisco, about 25 miles west of the city of Pinar del Rio on the Western Railroad of Havana. The principal ridges are anticlines, and consist of very thick deposits of sandy shales and slates containing a large number of little veins of white quartz which, by the gradual disintegration of the mass of the material, is left covering the surface. This quartz occasionally shows sulphide, but is generally barren of any such indication. At times lenticular masses of a more or less pure limestone were observed in these slates. The shales, which are of light color, are occasionally talcose. The formation would tentatively be classed as the Lower Cambrian, and the heavy ridges of comparatively horizontal limestone found in the anticlinal valleys as the Upper Cambrian. Along the crest of these slaty ridges deposits of iron-ore are found which are apparently in place, and were probably formed by replacement of masses of limestone similar to those noted elsewhere. The ready disintegration of the slates, and the

Jul 1, 1907

I. PRESIDING OFFICERS. At all Business meetings of the Institute the President, or, in his absence, the Vice-President, or, in the absence of both of them, any other member of the Board of Directors to be chosen by the meeting, shall preside. At all other meetings of the Institute the President of the Council or, in his absence, one of the Vice-Presidents, if present, shall preside II. ORDER OF BUSINESS. At each Business meeting of the Institute the order of business shall be as follows 1. Reading of minutes of preceding meeting. 2 Report of the President. 3. Report of the Treasurer. 4. Report of the Secretary. 5. Election of Directors. 6. Election of Members of the Council. 7. Reports of Standing Committees. 8. Reports of Special Committees. 9. Special Orders 10. Miscellaneous business. This order of business may be changed by a vote of a majority of the Members and Associates present in person or by proxy. The usual parliamentary rules shall govern all meetings of the Institute except in cases otherwise provided by the Constitution or the By-Laws. At all sessions of the Institute other than business meetings, the order of proceedings and the time of adjournment, shall rest in the discretion of the presiding officer

Jan 1, 1917

By Joseph E Pogue

Over a period of years the writer has presented a number of studies1 on various aspects of proration, in a progressive attempt to analyze critically and constructively the economic complexities of this interesting institution, which in a decade has revolutionized the economics of oil production in the United States. In the course of the investigations leading to these papers, the changing nature of proration and the principles underlying its evolution have gradually become clear, so that it is now possible to depart from the analytical method and to construct a synthesis of the steps that, if furthered by the industry, should carry proration past the economic hazards that still surround it to the goal of maximizing the value of the petroleum resource to the industry and the public alike. Nature of Proration Proration literally means the allocation of demand among competing producers on a pro rata basis, but the term now carries a much broader significance for it is employed to describe the entire process by which the production of crude oil in the United States is regulated. There is naturally much confusion of thought on the subject, for proration is an evolving system of control based upon principles of conservation and equity and embracing a body of practices that are tending to adjust themselves to the needs of the situation but are subjected to varying and divergent influences in the process. As it is now constituted, proration is a planned production measure designed to prevent waste, insure ratable takings, and balance supply and demand. The procedure is administered by State regulatory bodies through use of the police power of the States under authority of State conservation laws; the practice is supported by a considerable degree of voluntary conformance on the part of operators; and the Federal Government has accorded its cooperation by providing advisory quotas, circumscribing imports, checking movements of hot

Jan 1, 1939

By Joseph E. Pogue

Over a period of years the writer has presented a number of studies1 on various aspects of proration, in a progressive attempt to analyze critically and constructively the economic complexities of this interesting institution, which in a decade has revolutionized the economics of oil production in the United States. In the course of the investigations leading to these papers, the changing nature of proration and the principles underlying its evolution have gradually become clear, so that it is now possible to depart from the analytical method and to construct a synthesis of the steps that, if furthered by the industry, should carry proration past the economic hazards that still surround it to the goal of maximizing the value of the petroleum resource to the industry and the public alike. Nature of Proration Proration literally means the allocation of demand among competing producers on a pro rata basis, but the term now carries a much broader significance for it is employed to describe the entire process by which the production of crude oil in the United States is regulated. There is naturally much confusion of thought on the subject, for proration is an evolving system of control based upon principles of conservation and equity and embracing a body of practices that are tending to adjust themselves to the needs of the situation but are subjected to varying and divergent influences in the process. As it is now constituted, proration is a planned production measure designed to prevent waste, insure ratable takings, and balance supply and demand. The procedure is administered by State regulatory bodies through use of the police power of the States under authority of State conservation laws; the practice is supported by a considerable degree of voluntary conformance on the part of operators; and the Federal Government has accorded its cooperation by providing advisory quotas, circumscribing imports, checking movements of hot

Jan 1, 1939

By J. E. Chappelear

We are concerned with the problem of calculating the forces produced by passing waves on a submerged object (in particular a drilling barge) located on the ocean floor. We employ the linearized theory of waves (the Airy1 theory), since solutions are generally more easily obtained in such a theory. It will be indicated how an approximate solution to the problem can be obtained for waves of finite height by use of a linear combination of Airy waves. We shall assume the submerged object has an infinite length, thus neglecting diffraction and making the problem two-dimensional. We find that there is not a considerable difference between our solution and the usual engineering solution. The force, as a function of time, is plotted in Figs. 4 and 5, together with the usual solution for easy comparison. So far, no experiments have been found to compare with the results. As will be shown, the calculations can be extended to waves of finite height (Stokes2-Struik3 waves) in an approximate fashion. This can be done by calculating the force produced by each Fourier component of the wave, separately, and omitting the coupling between the various harmonics produced by Bernoulli's theorem. The problem and its boundary conditions will be briefly stated. We seek a function, +, the velocity potential, which is harmonic, ?2?=0...........(1) and which satisfies the boundary conditions ??/?n =0 .......(2) (the normal derivative of + is zero) on the ocean floor and the sides of the barge, and s??/?y = ?..........(3) on the ocean surface, where s = g/w2........(4) The physical reasons for these choices and an interpretation of ? are given by Lamb.' As previously stated, we assume also that the problem is two-dimensional. We set up our coordinates such that x = 0 is the center of the barge and y = 0 is the ocean floor. The coordinates are shown in Fig. 1, together with the location of the barge on the bottom. Our solution may be decomposed into a function which is symmetric about x = 0,?e, and one which is antisymmetric, +,, ? = ? + ?o...........(5) Thus directly above the barge we have as boundary conditions that for x = 0, ?o = 0, ...........(6) and ??e/?x = 0........(7) Now, far from the barge, we have that (for x positive and assuming the waves are incident from the left) ?e ? Ae cosh ky cos k (x + a) , . . . (8) and ?e ? Ao cosh ky cos k (x + ß) . . . . (9) where + means ". .. approaches ... for x large." Let us put Ae, Ao, and k equal to one, and remember that, in accordance with the derivation of Eq. 3, a sinusoidal time factor is to be supplied. Then we may rewrite Eq. 8 for ?e, and we find that

Jan 1, 1958

By R. A. Greenkorn

This project originated in a practical problem—we needed five tracers that could be used together to locate flow paths in a pilot flood. While tracers for subsurface liquids have been used since the turn of the century,1-15 none of those reported in the literature appeared to be either consistent or quantitative enough for our purposes. Most were used in field systems without controlled experiments to determine the accuracy and precision of analysis, and many were tracers that could not be used collectively. The ideal tracer, of course, would follow the fiuid of interest exactly, traveling at the same velocity as the fluid front. But the ideal is impractical to attain because adsorption-desorption effects cause the tracer to lag behind the front; these effects, plus diffusion-dispersion effects, cause the tracer front to spread more than the fluid front. Thus, our objective was not to locate a tracer that would be ideal for all circumstances but rather, to find one that would approximately follow the fluid, or one that under controlled conditions could be corrected to calculate the movement of the fluid front. We considered tracers satisfactory—(1) if they were easy to analyze; (2) if their breakthrough-elution curves were not too different from those for the chloride ion, a tracer believed to follow the fluid front closely; and (3) if we could calculate from the curves a material balance, at 1.25-PV (pore volume) injected, within 5 per cent of that calculated from chloride curves. Of a possible 35 materials, we selected 13 tracers that could be quickly and easily identified and whose analysis was claimed to be accurate within 5 per cent. Only one of these, tritiated water, was a radioactive tracer. Radioactive tracers are easy to detect even in small quantities, but they require special handling and special equipment. Also, those that can be used together are limited because special equipment is required to separate emissions from the various tracers. Two of the original 13 tracers were eliminated in static tests to determine how accurately and precisely they could be analyzed, and to check on gross adsorption. The remaining 11 were flowed through a 9-ft linear sandstone model, and breakthrough-elution curves were obtained. Finally, three tracers were field-tested as breakthrough tracers. These tests are described in the following sections. The 13 tracers considered in these experiments were EDTA (ethylene diamine tetra acetic acid), fluo-rescein, picric acid, salicylic acid and ammonium, boron (as borate), bromide, dichromate, iodide, nitrate and thiocyanate ions, plus chloride ion and tritiated water. All but the chloride ion and tritiated water were subjected to static sand tests to eliminate the tracers that could not be analyzed quickly and accurately and to eliminate those that showed excessive adsorption. All but two of the tracers, EDTA and salicylic acid, qualified for flow tests on this basis. The procedures used in the static tests (see Appendix A for analytical details) were as follows. Each tracer (in the amount shown in Table 1) was dissolved in 1,000 ml of water. Then, 800 ml of this solution was added to 500 gm of sand, and the remaining 200 ml was reserved as a control standard. The sand-tracer mixture was agitated once a day over a 10-week period, and during this period we analyzed five duplicate samples from this mixture, along with five duplicate samples from the control solution. From the control-sample analyses, we constructed a control chart on which the sand-tracer analysis results were plotted. The control chart, and its use to determine accuracy and precision of analytical results, as well as the amount of adsorption, is described in Appendix B. The results of the static tests are summarized in Table 1, which lists the concentration c (concentration at time t) divided by c, (initial concentration). If there was no adsorption, c/c, = 1. The acceptable deviation from this value varied from tracer to tracer, depending upon the limits of analytical precision established for the different tracers. The best results were obtained with boron, bromide and dichromate, with all values falling within limits of accuracy and precision. Ammonium, iodide, nitrate and picric acid also were satisfactory, although the ammonium results were erratic. Flourescein and thiocyanate were unsatisfactory ini-

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