The following article was written by George Vander Voort to commemorate the 75th anniversary of the founding of ASTM Committee E-4 on Metallography. It describes the history of ASTM Committee E-4 from 1916, when it was organized, to 1991 when the article was written. It originally appeared in ASTM Standardization News, May, 1991 as "75 Years of Metallography, The ASTM Committee E-4 Perspective" and is reproduced here with the kind permission of Mr. Philip Lively, assistant VP for publications, marketing, and information technology at ASTM.
ASTM Committee E-4 on Metallography, organized on Oct. 10, 1916, grew out of Committee E-1 on Methods of Testing (as is true of many other "E" committees). At that time, standard E1-16, Methods of Testing (originally adopted in 1910) consisted of five parts, the last entitled "Methods for Metallographic Tests of Metals" requiring somewhat less than three pages. The organizational efforts were chaired by Edgar Marburg, ASTM's Secretary-Treasurer, who died in 1918.
At that time, it was perceived that there was a need to establish standard magnifications for micrographs and that this work would be best performed by a new standing committee. This new group was called Committee E-4 on Magnification Scales for Micrographs. Actually, there had been an earlier committee called E-4 on Methods of Sampling and Analysis of Coal, which was disbanded in 1915, and there also was a disbanded E-3 at the time. Hence, we could have been known as E-3 on Metallography just as easily as E-4. At any rate, the original E-4 name did not last long because the members realized that the establishment of standard magnifications was a simple task and many more complex problems needed to be solved. Subsequently, in 1920, the members decided to change their name to Committee E-4 on Metallography, and this name has been used since 1921. Committee E-4's original 15 members, not counting Marburg, listed two ASTM presidents, Dr. Henry Marion Howe, the dean of American metallurgists at that time, and George Kimball Burgess, famed director of the National Bureau of Standards. Howe was a founder of ASTM, his name is the first listed on the charter, and he was the first ASTM president (see biographical sidebar on his many accomplishments)(Webmasters note: accompanying sidebars will be posted soon).
Committee E-4, as with all volunteer groups, has had its share of successes and failures. History will judge the committee based mainly on its tangible accomplishments. These can be viewed in several ways. Issuance of standards is an obvious yardstick; E-4 has published 42 standards (see sidebar, E-4 Standards at a Glance)(Webmasters note: accompanying sidebars will be posted soon). Of these, seven were discontinued (six of these were replaced by newer documents), five were transferred to other standing committees and 30 are now active. Another good yardstick is symposia, particularly those subsequently published. E-4 has sponsored or co-sponsored numerous symposia since 1936. These have generated 24 ASTM Special Technical Publications (STPS) (see sidebar)(Webmasters note: accompanying sidebars will be posted soon). Two other E committees, E-7 on Nondestructive Testing and E-37 on Thermal Measurements, were spun off E-4 and have been highly successful. E-4 members started the highly significant work of the joint Committee on Powder Diffraction Standards, JCPDS, in Swarthmore, PA, and four E-4 members have been officers of this organization. Four E-4 members have served as vice-president and five as president of ASTM and eight others have served as directors or as members of the executive committee. Thirteen E-4 members were made honorary ASTM members and 34 have received the Award of Merit (five were made Fellows prior to creation of the Award of Merit). Naturally, some of these men were also active on other committees. (A sidebar lists E-4 award winners.) (Webmasters note: accompanying sidebars will be posted soon)E-4 members have been active in other societies, for example, nine E-4 members have been presidents of the American Society for Metals.
It is more difficult, however, to gauge how well Committee E-4 has served the metallographic needs of industry. Has E-4 met the needs of the metallographic community in a timely fashion? Have other groups done a better job? Has E-4 lead the way in standards development compared to other technical societies, here or abroad, or industrial companies? These are tough questions to answer, but a Iittle soul searching is necessary at times. In general, we would conclude that E-4 has done a very good job overall, as ASTM metallographic standards are the most widely used in the U.S. and many other countries have followed our lead. No doubt we could have been faster in many of our tasks. (Of course, this is a totally unbiased, highly precise evaluation, based upon a massive survey - of one!) But, as Paul Harvey says, let's hear "the rest of the story!"
Committee E-4 has met at least 137 times since its formation. This May's meeting will be the 31st in Atlantic City, NJ, the last being in June of 1971. Philadelphia, New York, Pittsburgh, and Chicago were the next most frequent meeting sites with 16, 10, 9, and 8 visits, respectively. Committee E-4 membership (see Figure 1)(Webmasters note: accompanying Figures will be posted soon) grew steadily over the years, reaching its peak in 1979 with 161 members. Since then, membership has been declining steadily. These numbers are somewhat deceptive as some of the members were consultants (non-dues paying) and for the past ten years we have been purging the roster of members who do not return ballots. However, compared to the peak years, E-4 has had a reduction in active meeting participants. This trend is not unique to E-4.
Despite this, Figure 2 (Webmasters note: accompanying Figures will be posted soon)shows that E-4's standards development effort has not decreased, but increased. In 1979, E-4 had 15 active standards. In the last 11 years, this number has doubled to 30 (see sidebar)(Webmasters note: accompanying sidebars will be posted soon). Prior to 1979, E-4 had developed 24 standards but nine were either transferred to other committees, discontinued, merged with another, or replaced. Since 1979, 17 new standards have been developed, one was transferred and one was replaced by a new standard. Either way, the past eleven years have been highly productive despite the loss of E-4 membership.
Only 13 people have chaired Committee E-4 (see Table 2) (Webmasters note: accompanying Tables will be posted soon), largely because LeRoy L. Wyman, Sr. (see biography)(Webmasters note: accompanying biography will be posted soon) held the chairmanship for 28 years (1938-1966), an ASTM record. However, E-4 was not the only committee Wyman chaired. (Wyman certainly could qualify as a full-time, unpaid ASTM employee!) More recently, Committee E-4 chairmen have been restricted to no more than two consecutive two-year terms.
There have been 13 E-4 secretaries, the first elected in 1921. Three people held this position for long periods: Mary R. Norton (20 years), John J. Bowman (ten years), and George F. Comstock (nine years). In 1936, E-4 appointed its first vice-chairman, Dr. Marcus A. Grossman, who held the position for eight years. Grossman was internationally recognized for his work in hardenability. He was followed by R. Earl Penrod (see biography) (Webmasters note: accompanying biography will be posted soon)who held the position for 20 years. Wyman, Penrod, and Norton ran Committee E-4 for about a third of its existence! E-4 also has the unique distinction of having father and son chairmen, William D. Forgeng, Sr. and Jr. (see biographies)(Webmasters note: accompanying biographies will be posted soon), serving with only a two year gap between them.
Committee E-4 appointed its first second vice-chairman in 1972 and eight people have held this position for either two- or four-year terms. Our first membership chairman was appointed in 1964 and eight people have served in this capacity. (A sidebar lists all of the past E-4 officers and their terms of office.)(Webmasters note: accompanying sidebars will be posted soon)
Committee E-4 created 15 subcommittees, with the first started in 1920. Roman numerals were used to number subcommittees up until 1970, since then Arabic numbers have been used. (In this text, Roman numerals are used when referring to a sub and its activities before 1970 and Arabic numbers for subsequent events.) Only eight subcommittees are now active, mainly due to mergers. See the sidebar for a list of all the past E-4 subcommittee chairmen and their terms of office.(Webmasters note: accompanying sidebars will be posted soon)
Sub 1 on Sample Selection and Preparation and Photography was formed in 1920 as Sub I on Preparation of Metallographic Specimens. Its name was changed twice, in 1921 and 1988, the latter due to the merging of Sub 4 on Photography into Sub 1. When many people think of metallography, they think of Sub l's domain first. Indeed, Sub l's activities have always been a focal point of E-4 concentration. Sub 1 has prepared the greatest number of standards and has jurisdiction over eight active standards, the most of any E-4 subcommittee. Sub 1 has had ten chairmen with one person, Sam Purdy, serving during two different time periods for a total of 23 years (and still going strong!). The list of Sub 1 chairmen is very impressive.
For many years, standard E 2, Methods for Preparation of Micrographs of Metals and Alloys, guided metallographers but it was discontinued in 1983 at the age of 66. The original version, introduced in 1917 (they were off to a good start) and written largely by William H. Bassett of American Brass Co. (see biography)(Webmasters note: accompanying biographies will be posted soon), contained grain size measurement information, which really was inconsistent with the specification title, until 1949, when this information was removed and incorporated into new standard E 79, Methods for Estimating the Average Grain Size of Wrought Copper and Copper-Base Alloys. Methods E 2 also had the first grain size chart for copper, added in the 1930 revision. This chart was developed by Edgar H. Dix, Jr., Francis F. Lucas, Henry S. Rawdon, and Charles H. Davis. The actual micrographs were prepared by Davis and his staff of the American Brass Co. in Waterbury, CT.
Standard E 3, Methods for Preparation of Metallographic Specimens, has been one of the most important E-4 documents. In the early days of this century, there were few, if any, compilations of preparation procedures and etchants. Methods E 3, prepared largely by Henry Marion Howe, pulled much of the existing information together and this was continually updated. E. C. Groesbeck of the then U.S. Bureau of Standards and a developer of selective etchants contributed to this work.1
In 1928, Sub 1 introduced metallographers to the use of Bakelite (phenolic plastic) for mounting specimens. Later, in 1938, LeRoy L. Wyman presented a detailed report on the use of plastics for mounting.2 In 1932, Wyman replaced William E. Ruder as General Electric Research Laboratories representative, thus beginning a long, productive association.
Throughout the 1920s and 1930s, Sub 1 was constantly searching for sources of good cloths for polishing. Wyman reported that due to fashion changes in the 1920s, "kitten-ear" broadcloth, a very popular polishing cloth, had become unavailable.3 Wyman canvassed the garment district of New York City for possible substitutes. E-4 members tried these but without success. Eventually, they persuaded the Horne Co. of Pittsburgh to produce kitten ear for metallographers. ASTM was convinced to order huge rolls of this cloth which was sold to metallographers at cost. After several years in the polishing cloth business, a newly formed metallographic supply house took over this function. Kitten-ear cloth is still commonly used for final polishing of soft metals where scratch removal is particularly difficult.
With each revision, standard Methods E 3 grew and grew, from the initial 13-page 1921 version to a 66-page document in 1958. At this time, it was felt that Methods E 3 was becoming cumbersome. Information on macroetch and microetch compositions and uses was removed from Methods E 3 and used as the basis for new standards Method E 340, for Macroetching Metals and Alloys, and Methods E 407, for Microetching Metals and Alloys, respectively. In 1980, Methods E 3 was reduced to coverage of mechanical polishing alone. Subsequently, standard E 1180, Practice for Preparing Sulfur Prints for Macrostructural Examination, was written expanding upon the brief description of sulfur printing found in Methods E 3 up to 1980. The electropolishing information in Methods E 3 up to 1980 has not yet emerged as a new standard but this work is again moving forward.
Sub I developed standard E 381, Method of Macroetch Testing, Inspection, and Rating Steel Products, Comprising Bars, Billets, Blooms, and Forgings, building upon ASTM A 317, Method of Macroetch Testing and Inspection of Forgings, to describe classification and interpretation of macroetched sections cut from wrought ingot-cast material (blooms, billets and bars, for example). This is a general purpose standard that complements other special purpose standards, e.g., A 561, Practice for Macroetch Testing of Tool Steel Bars, and A 604, Method for Macroetch Testing of Consumable Electrode Remelted Steel Bars and Billets. Continuous casting has become increasingly popular due primarily to cost savings. Steels made by this process may be evaluated for macrostructure in the as-cast condition, unlike ingot cast material, or after hot reduction. The existing Method E 381 macroetch classification charts are not really useful for continuously cast steels, particularly if tested in the as-cast condition. An extensive effort has been under way for several years now to expand Method E 381's coverage.
Another recent effort of Sub I has been the development of E 1351, Practice for Production and Evaluation of Field Metallographic Replicas, which describes how to make and evaluate replicas made in the field to estimate the remaining life of steam piping in power plants. This standard began life as an emergency standard, ES 12, Practice for Production and Evaluation of Field Metallographic Replicas, E-4's only emergency standard. This approach was taken as a result of a serious accident due to failure of a main steam line. Many power plants are now at or beyond their original design life. Assessment of the remnant life of components subjected to many years of high temperatures and pressures has relied upon examination of microstructural evolution and the formation and growth of creep cavities under these operating conditions. Almost over- night, numerous people were involved in such evaluations and there was an obvious need to standardize the procedures. Sub 1 was approached by members of the power generation industry to tackle this problem and they responded swiftly with a highly useful document. Sub 1 is now working on preparation methods for thermally-sprayed coatings.
Sub 2 on Metallographic Terminology and Nomenclature of Phase Diagrams was formed in 1920. Originally, definitions were to be incorporated into Methods E 2 and 16 terms were first defined and balloted. However, only eleven of these made it through the ballot process and a separate standard, E 7, Definitions of Terms Relating to Metallography, was issued in 1924. it was soon noted that Committee E-4 on Metallography had forgotten to define metallography so this term was added in 1926, revised in 1927.
Henry C. Boynton was Sub II's first chairman and Professor Arthur Phillips of Yale Univ, was the second. Initially called Sub II on Nomenclature and Definitions, it was inactive through most of the 1930s. Reactivated under Dr. Robert S. Williams of the Massachusetts Institute of Technology in 1939, it stayed active only two years, as he recommended against revisions to Definitions E 7.
In 1946, efforts were made to revise Sub II but nothing happened until 1948, when Dr. Paul A. Beck of Notre Dame (later of the University of Illinois) was appointed chairman. The sub was renamed Sub II on Definitions and Beck started a massive effort to turn Definitions E 7 into a comprehensive terminology standard. Beck created a long list of potential terms and turned this work over to Dr. Robert S. Busk of Dow Chemical Co. Nearly 1,000 terms were considered. In 1955, Definitions E 7 jumped from 12 definitions to a 45-page document with 750 definitions.
After this massive effort, Sub II became inactive in the late 1950s until 1966, when Mary R. Norton of Watertown Arsenal (see biography)(Webmasters note: accompanying biography will be posted soon) became chairman. She worked with then Committee E-8 on Nomenclature and Definitions to add metallography terms to the new ASTM glossary. She also worked with members of new Committee E-25 on Microscopy to compare definitions for the same terms in Definitions E 7 and in their terminology standard, E 175, Definitions of Terms Relating to Microscopy. This revealed 23 definitions with differences to be reconciled, which was done. Since 1955, there have been at least 13 additional revisions of Definitions E 7 involving refinements to definitions, deletions of obsolete terms, and additions of new terms, e.g., on electron metallography and image analysis. More recently, Sub 2 has been working on adding symbol and acronym sections.
Sub 3, formed in 1920 as Sub III on Thermal Analysis, has had an interesting history. In 1920, E-4 recommended to ASTM that a standard committee be formed on pyrometry as this was too far outside the scope of E-4. While temperature measurement per se was considered too far afield, the interpretation of cooling curves and thermal arrests were not. In the early days of metallography, one of the chief activities was the construction of equilibrium phase diagrams; thermal analyses (both heating and cooling) was a major tool for such work.
The first chairman of Sub III was George Kimball Burgess, director of the U.S. Bureau of Standards who was replaced, after a few years of inactivity, by William E. Ruder of General Electric Co. Ruder and his subcommittee produced standard E 14, Practice for Thermal Analysis of Steel, in 1925. This standard was revised five times and then transferred to new Committee E-37 on Thermal Measurements in 1978. Howard Scott took over Sub III in 1928, but activity stopped by 1933.
In 1949, this committee was reactivated as Sub III on Nomenclature under Dr. Paul A. Beck. Its goal was to establish a system of nomenclature for alloy phases in binary and more complex systems. The development and construction of equilibrium phase diagrams was not standardized and the naming of phases was performed erratically. Beck pulled together a subcommittee consisting of the major American and British experts on phase diagrams (not all were ASTM members)-K. W. Andrews, Max Hansen, William Hume-Rothery, F. Laves, Taylor Lyman, John S. Marsh, G. V. Raynor, Frederick N. Rhines, Cyril Stanley Smith and Arthur J. C. Wilson, besides knowledgeable E-4 members such as Robert S. Busk and William L. Fink. The latter became the subchairman in 1960 and held this position until 1978.
This work, started by Beck and continued by Fink, resulted in a new system of alloy phase nomenclature described in standard E 157, Method for Assigning Crystallographic Phase Designations in Metallic Systems, introduced in 1961. 4,5The subcommittee then began work on rules for drawing phase diagrams suitable for publication. This resulted in standard E 391, Practice for Presentation of Phase Diagrams, in 1969. Since then, aside from revisions to Method E 157 and Practice E 391, which have been minor, there has been no activity in this area and Sub 3 was merged into Sub 2 in 1988.
Sub IV on Photography was also established in 1920. V. H. Bihlman was the first chairman, followed by Henry S. Rawdon and Leon V. Foster, each of whom served for long periods (I2 and 17 years, respectively). Foster developed the well-known, very popular calcite prism polarizer used on Bausch and Lomb metallographs. Sub IV developed photomicroscopy information that was incorporated into standard Methods E 2. The introduction of E 883, Guide for Metallographic Photomicrography in 1983, which was a massive updating of the photographic information formerly in Methods E 2, lead by Fran Warmuth, resulted in the withdrawal of Methods E 2.
One of Sub IV's most significant achievements was the sponsorship of the annual ASTM photographic contest, which started in 1936 but ended with the 1980 contest. The decision to stop the society-wide annual meeting made it very difficult to run the contest. Sub IV also held a symposium in 1948 on the use of color in photomicroscopy (STP 86, Symposium on Metallography in Color). At that time, such use of color was in its infancy and the symposium demonstrated the value of color. After the issuance of Guide E 883, and the demise of the annual photographic contest, Sub 4 activity waned. In 1988, Sub 4 duties were taken over by Sub 1.
Sub 5 on Microindentation Hardness Testing was created in 1923 as Sub V on Micro-Hardness to evaluate the scratch hardness instrument developed by C. H. Bierbaum, an E-4 member. Henry S. Rawdon chaired the committee. The method was found to be usefuI only in a comparative manner to show differences in hardness between different constituents.6As no other microindentation equipment existed at that time, the sub was disbanded in 1927.
Instrumentation, using both Knoop and Vickers type indenters, was developed starting in the late 1930s, prompting E-4 to reactivate the committee, now Sub V on Microhardness, in 1948 under Alexander Gobus. A round robin (the first of many) was initiated in 1950 to evaluate instruments. At the request of Sub V, Bausch and Lomb developed a new stage micrometer in 1950 with 0.02 um accuracy.
Walter A. Shebest of the Frankford Arsenal took over Sub V in 1955 and the round robin continued. After a period of inactivity, Larry Toman, Jr. took over Sub V in 1965. One of his first tasks was to define microhardness. Today, E-4 tries to discourage use of this term although its use is thoroughly ingrained. Microhardness, at face value, suggests a very small hardness, which is not the intention. These tests produce a very small indentation due to application of a rather low load, to determine the same hardness number (hopefully) as obtained using a bulk test with a much higher load and much larger indent. Consequently, the preferred term is microindentation hardness testing.
Toman and Sub V issued standard E 384, Method of Test for Microhardness of Materials, in 1969 to cover Knoop and Vickers microindentation testing. In 1975, the symbols HV and HK were adopted in preference to the original VHN (or DPN) and KHN. Another round robin was begun in the late 1970s, but it was dropped after only four laboratories completed the tests. It was apparent that the approach used was too complex. The resuIts appeared to show that most of the variability of test results occurred in the measurement of the indents, rather than in making the indents.
Yet another round robin was begun in the early 1980s. Seven test blocks, three ferrous and four nonferrous, were indented by one person using five indents at each of six loads, with both Knoop and Vickers indenters. The ferrous and nonferrous test specimens were separated and sent to different companies. Twelve people measured the indents on the nonferrous specimens and 14 people (24 different people in all) measured indents on the ferrous specimens. Tony DeBellis tabulated all of the test results but analysis work was slow in coming. This writer agreed to evaluate the ferrous data. After this was done, and the nonferrous data was still untouched, I again volunteered. The results of this round robin (its origins can be traced back at least to 1972) were used to prepare a detailed precision and bias section for Method E 384 . 7,8
Sub VI on X-Ray Crystal Analysis was started in 1924. The eminent metallurgist Zay Jeffries was its first chairman. Jeffries became interested in the new field of X-ray diffraction after World War I when acting as a consultant to the Cleveland Wire Co. of General Electric Co.9 He hired a young metallurgist, Edgar Collins Bain (who later gained fame and fortune with the United States Steel Corp.), to evaluate these new techniques.10
The initial work of Sub VI consisted of introduction of standard E 15, Methods of Radiographic Testing of Metal Casting, written by Horace H. Lester of the Watertown Arsenal in 1926, publication of a glossary of X-ray metallography terms11 prepared by Louis W. McKeehan of Bell Telephone Laboratory (later at Yale Univ.), and issuance of a superb review paper12 on the current status of X-ray metallography (prepared by Jeffries, Lester, McKeehan and Bain).
In 1931, the name was changed to Sub VI on X-Ray Methods and in 1933, Dr. Robert F. Mehl of the Carnegie Institute of Technology (now Carnegie Mellon Univ.) became chairman. Mehl played a dominant role in the founding of the science of physical metallurgy. His main contribution as an E-4 member was the organization of E-4's first symposium, held on July 2, 1936, on Radiography and X-Ray Diffraction Methods which became E-4's first STP (STP 28, Symposium on Radiography and X-Ray Diffraction Methods). At that time, X-ray diffraction was unlocking the secrets of metal crystals. It was the first really powerful tool for studying the internal structure of crystalline materials.
In 1937, E-4 recommended that a separate standing committee be formed to cover the inspection aspects of X-ray methods, i.e., radiography. Subsequently, Committee E-7 on Radiographic Testing (now E-7 on Nondestructive Testing) was founded in 1938 under the chairmanship of Horace Hardy Lester. 13 Methods E 15 was transferred to Committee E-7 in 1939.
William L. Fink of Alcoa took over Sub VI in 1938 and continued as subchairman until 1960. Under Fink, standards E 43, Practice for Identification of Crystalline Materials by the Hanawalt X-Ray Method; E 81, Method for Preparing Quantitative Pole Figures of Metals; and E 82, Method for Determining the Orientation of a Metal Crystal, were developed. In 1940, Sub VI began perhaps its greatest task, the establishment of a center for information on diffraction methods for chemical analysis. in 1941, they began work with an X-ray diffraction group of the National Research Council, providing the technical expertise and personnel to start a file catalog of materials already identified by X-ray diffraction. Within a year, 250 sets of X-ray file cards with 3,936 entries had been prepared.
This effort spawned the Joint Committee on Powder Diffraction Standards (JCPDS) in Swarthmore, PA, now jointly co-sponsored by a number of organizations worldwide.14 Their function has been to collect, edit, publish, and distribute powder diffraction data. Solids were first studied by X-ray diffraction in 1912; A. W. Hull (General Electric Co.) reported the need for a database of diffraction patterns in 1919. Hull demonstrated the unique nature of each crystalline substance's diffraction pattern, which did not change, even when several substances were mixed together. Development of a diffraction pattern file was hampered by the fact that they were recorded on a photographic negative. A classification scheme for the films was developed in 1936 and published in 1939 by Joseph D. Hanawalt, Harold W. Rinn, and L. K. Frevel of Dow Chemical Co.15 This paper began the cataloging effort as diffraction patterns for 1,000 substances were tabulated.
Sub VI and the National Research Council (NRC) formed a joint committee, joined shortly by the institute of Physics of Britain who supplied a number of diffraction patterns. NRC was replaced by the American Society of X-Ray and Electron Diffraction (now the American Crystallographic Society) and other groups have since joined. JCPDS was housed initially at Pennsylvania State Univ. in the office of E-4 member and first JCPDS chairman, Dr. Wheeler P. Davey. It has been located in Swarthmore since 1970.
The original method for searching the database has changed somewhat as the files have grown. Hanawalt revised his original method to one based on the three strongest peaks. This was later modified by William L. Fink to a system of ordering and reordering of the eight strongest peaks. As the files continued to grow, hand searching became tedious and other methods have been tried, e.g., visual comparative search systems .16-18 Despite the magnitude of the file now, the information can be obtained in printed form and on microfiche. X-ray diffractometers can be equipped with the entire powder diffraction file on a CD-ROM for rapid computer searching. Besides JCPDS's massive effort to collect diffraction data published worldwide, it also evaluates the quality of the data - a challenging task! E-4 members Wheeler P. Davey, William L. Fink, LeRoy L. Wyman, and Andrew W. Danko have served as chairman and/or general manager of the JCPDS.
Not all of Sub VI's efforts have been this successful. In 1942, Practice E 43, covering the Hanawalt method for identifying substances by X-ray diffraction, was issued. It was intended to be a companion to the new joint committee powder diffraction database. Practice E 43 was revised twice, in 1946 and 1949. Thereafter it was under a constant state of revision, even up to seven years after it was withdrawn (in 1961). The subject was considered to be too complex for a standard and a book was started but never completed.
More recent years have seen the development of an X-ray diffraction standard for measuring the retained austenite content of steels, written mainly by Robert W. Hinton of Bethlehem Steel Corp., and issued in 1984. Since then, activity has decreased and Sub 6 became inactive in 1987, then merged into Sub 11.
Sub VII on Recommended Practice for Dilatometric Analysis was formed in 1938 with LeRoy Wyman, chairman of Committee E-4, as subchairman as well. Laurence H. Carr (Edward Valves, Inc.) took over from Wyman in 1940 and ran Sub VII for the next eleven years, during which standard E 80, Practice for Dilatometric Analysis of Metallic Materials, was developed and issued in 1949. Practice E 80 was reapproved but not revised through 1978 when jurisdiction was transferred to Committee E-37.
Donald I. Finch of Leeds & Northrup Co. took over Sub VII in 1951 and ran it for the next 19 years. During his tenure, standard E 189 Practice for Determining Temperature-Electrical Resistance Characteristics of Metallic Materials, was developed and issued in 1961. As with Practice E 80, it was transferred to Committee E-37 in 1978.
Committee E-4 has always been active in the area of grain size measurement (WebMaster's note:see article) but a separate committee was not established until 1931. This work was assigned to a Special Committee on Grain Characteristics, rather than a subcommittee, with Clarence J. Tobin of General Motors Research Laboratory as its chairman. Their first effort was to develop a procedure for assessing the grain growth characteristics of a given heat of steel. The method chosen was the McQuaid-Ehn carburizing test originally developed to assess the suitability of a low-carbon steel for carburizing. Harry McQuaid of Republic Steel Corp. was a consulting member. A chart was developed depicting the hypereutectoid and hypoeutectoid regions of the carburized case of specimens with different grain sizes; the method and chart were issued as standard E l9, Classification of Austenite Grain Size in Steels, in 1933.
In 1937, Dr. Marcus A. Grossman took over the Special Subcommittee which became Sub VIII on Grain Size in 1938. Although Classification E 19 was an important development, and the original chart was claimed to be a result of ten years effort, the chart was widely criticized as inaccurate and was under constant revision up to 1961 when it was withdrawn. Grossman formed three separate groups under Sub VIII. Group A was to revise Classification E 19 and he headed it. Group B was to develop a ferrite grain size rating method and was headed by R. Earl Penrod. Group C was to develop methods for nonferrous alloys other than copper and was headed by Carl H. Samans of Standard Oil Co. of Indiana. H. P. George (Dept. of the Army-Frankford Arsenal) took over group C in 1951 and Penrod replaced Grossman after he died in 1952.
Their work resulted in three new standards, E 79, Methods for Estimating the Average Grain Size of Wrought Copper and Copper-Base Alloys, issued in 1949; E 89, Methods for Estimating the Average Ferrite Grain Size of Low-Carbon Steels, issued in 1950; and E 91, Method for Estimating the Average Grain Size of Non-Ferrous Metals, Other than Copper, and Their Alloys, issued in 1951. Methods E 79, however, was for copper-based alloys and was largely the grain size information stripped out of Methods E 2. This work revealed and confirmed comments from members that grain size analysis was basically a problem of geometry and a single standard could be developed for all alloys.19,20 For comparison ratings, it would be necessary to have charts developed that were realistic depictions of true structures. Standard E 112, Methods for Determining the Average Grain Size of Metals, grew from these ideas and replaced Classification E 19, Methods E 79, Practice E 89 and Method E 91, the latter three having rather short lives. The only grain size chart that survived was the copper chart of Methods E 79, but it too was modified. Today, Methods E 112 is one of the most widely cited ASTM test methods. Nothing, of course, is sacred. Methods E 112 has been revised 11 times in its 36-year history, with a twelfth revision underway. (Webmasters note: this revision has since been issued)The most significant revision to Methods E 112 occurred in 1974, when the three-circle intercept procedure, developed by Dr. Halle Abrams of Bethlehem Steel Corp., was added along with a statistical evaluation procedure to assess the quality of the measurements.21
While Methods E 112 contains extensive information about grain size measurement procedures, the most commonly used method is the chart comparison procedure. Numerous approaches have been suggested. For example, the appropriate chart can be placed on the wall and the operator examines the structure through the microscope eyepieces and then looks up at the chart. Reticles can also be prepared depicting portions of the grain size pictures and these can be superimposed over the image viewed through the eyepieces. Clear plastic templates of the grain size photographs can be placed over a projection screen. Charles H. Davis described a projection box device produced for the Bausch and Lomb Euscope for grain size rating.22 Frederick C. Hull of the Westinghouse Research Laboratories improved the comparison rating approach revealing factors that affect its precision and developing correction factors for using alternate magnifications. 23
Methods E 112 is used for rating the grain size of equiaxed grain structures. It has some guidance, currently being improved, for measuring deformed grain structures. However, other situations exist that are not covered. In certain metals and alloys, we sometimes observe a few grains, generally widely scattered, that are far larger in size than the rest of the grains. Standard E 930, Methods of Estimating the Largest Grain Observed in a Metallographic Section (ALA Grain Size), the ALA (as large as) method, describes how to measure these "rogue" grains. Methods E 930 was written by Robert Slepian and Fran Warmuth. It is also possible to have larger amounts of these mixtures, and a number of such patterns can be observed. Such specimens exhibit a non-Gaussian distribution of grain sizes and are referred to as bimodal or duplex. Standard E 1181, Test Methods for Characterizing Duplex Grain Size, written by Jeremy P. Morse, covers these situations.24
Sub IX on Inclusions was formed in 1940 and was chaired for 25 years by Samuel Epstein of Bethlehem Steel's Research Department until he retired. His six successors have served for the following 26 years. Epstein had developed an inclusion measurement method in his previous job at Battelle .25 Standard E 45, Practice for Determining the Inclusion Content of Steel, was issued in 1942 containing a chart rating method based on Swedish work and the non-chart method developed by Epstein. In 1960, a second chart method was added based on work by Walker and two years later, the third chart was added, the modified J-K chart for steels with low inclusion contents.26 Practice E 45, revised nine times, is also a widely referenced standard.
Sub IX also developed a standard practice for detecting large inclusions in bearing steels by ultrasonics, E 588, Practice for Detection of Large Inclusion in Bearing Quality Steel by the Ultrasonic Method.27 It was transferred to Committee E-7's jurisdiction in 1984. Sub 9 is presently evaluating the electron beam melt button test for rating the inclusion content of superalloys.
Sub X was not one of Committee E-4's big successes, either time it existed. Formed first in 1949 as Sub X on Decarburization, the sub members worked with the Society of Automotive Engineers (SAE) and the American Iron and Steel Institute (AISI) to develop a measurement method, but no E-4 standard resulted, activity stopped in 1952, and Sub X was disbanded in 1956. In 1968, it was reborn as Sub X on Research. Whatever the original purpose was, nothing of significance apparently resulted and Sub X was again disbanded. Sub X has two strikes against it, but it has not yet gotten to bat for a third time.
Sub XI on Electron Microstructure of Steels was formed in 1949. Its name has been changed seven times in the past 39 years, an E-4 record. Sub 11 has also had the most chairmen - 18 since 1950, another E-4 record. Sub 11 has also taken over the work of three other E-4 subs - Subs 6, 15, and 16. Sub 11 has sponsored more symposia and published more STPs than any other E-4 subcommittee. It has not been as prolific in developing standards, however, as it has only developed two: E 766, Practice for Calibrating the Magnification of SEM Using NBS-SRM 484, and E 986, Practice for Scanning Electron Microscopy Performance Characterization (both written by Dave Ballard of the National Bureau of Standards).
Sub 11 had its origins at the 1947 annual meeting of the Electron Microscope Society of America (EMSA), where discussions were held among transmission electron microscope enthusiasts working with metals. They formally organized a group on Feb. 13, 1948, and then merged their group into E-4 in 1949. Their first subchairman, George E. Pellissier of U.S. Steel Corp., was appointed in 1950. They were a fairly large, very active group and published seven detailed annual subcommittee reports in the 1950s before concentrating mainly on symposia for this purpose.
Electron microscopy was a hot topic in 1950 as the TEM provided at least an order of magnitude increase in resolution over the light microscope at that time. At that time, metal structures were only examined using replica methods; Sub XI did outstanding work in developing these procedures. Later, when thin foil methods were developed, Sub XI again played a major role in developing this method. Sub XI also produced a very popular manual on TEM techniques, STP 547, Manual on Electron Metallography Techniques.
While their initial work centered on ferrous alloys, Sub XI started a B group on nonferrous alloys in 1954, the same year they published their first symposium as STP 155, Symposium on Techniques for Electron Metallography. A C group on super strength alloys followed in 1956, and so did the STPs - STP 245, Advances in Electron Metallography, and STP 262, Symposium on Electron Metallography. In 1960, the C group topic was Electron Microstructure of PH (precipitation hardened) Austenitic and Ni-Based Alloys - a very active group. A group on Electron Diffraction followed in 1961, and another STP, STP 317, Symposium on Advances in Electron Metallography and Electron Probe Microanalysis. The electron microprobe analyzer was introduced and Sub XI got interested. A round robin was conducted on 316 stainless steel with former Committee A-10 on Iron-Chromium, Iron-Chromium-Nickel, and Related Alloys.
In October of 1966, Sub XI formed a task group (number 6, numbers being used now) on the Analysis of Extracted Phases in Superalloys under Matthew T. Donachie, Jr. of Pratt & Whitney Aircraft. This group became a special task group, TG 001, in 1968, then in 1975 a special subcommittee, E04.91, then in 1977, it became the only task group of a new subcommittee as E04.16.01, then Sub 16 was merged back into Sub 11 in 1983 and it was again a Sub 11 task group, completing a grand swing through E-4! On the way, they did issue (in 1983) a very fine standard, E 963, Practice for Electrolytic Extraction of Phases from Ni and Ni-Fe Base Superalloys Using a Hydrochloric-Methanol Electrolyte, which describes a method for extracting second phases from Ni-based superalloys. This task group was exceptionally active overthe 17 years; some of the results of their round robins are described in Refs. 28 and 29.
Another very active task group was TG 1115 on fiber analysis, chaired by Kuldip Chopra of ELKEM Metals Co. In the mid-1970s, there was a great deal of interest in contamination of water and air by asbestos fibers. However, there were no accepted methods established for sampling water, or air, and then for identification. There were individuals performing such work, for example, using polarized light examination, but the Federal laws being passed would require much greater testing and many new laboratories would be doing such work. New approaches were being examined, for example, energy-dispersive spectroscopy (EDS) using the relatively new scanning electron microscope (SEM) or electron diffraction (ED) using the transmission electron microscope (TEM). Clearly, there was a need to establish standards. The task group labored long and hard but, alas, no ASTM standard resulted, although a great deal of insight was developed.30
Sub 11's only standards (Practice E 963 was written before Sub 16 was merged back into Sub 11) have been in the area of scanning electron microscopy. The SEM was commercially introduced in 1965 and became an instant winner. Dave Ballard of the National Bureau of Standards (now a consultant) wrote two standards, Practice E 766 for SEM calibration3land Practice E 986 for SEM performance evaluation.32 In more recent times, Sub 11 has been conducting EDS round robins, organized by Frank Vetry of Inco Alloys Inc., and a draft for a guide to energy-dispersive X-ray analysis (EDXA) has been written by Dr. John J. Friel of Princeton Gamma-Tech..
Committee E-4 never had a Sub 12, no one seems to know why; and, Sub 13 has always been the name of our evening dinner activities at meetings, so we will jump to Sub XIV on Quantitative Metallography formed in 1960. As with Sub XI, George E. Pellissier of U.S. Steel Corp. was its first chairman. One of its first activities was to work with former Committee A-3 on Cast Iron on the graphite rating charts in standard A 247, Method for Evaluating the Microstructure of Graphite in Iron Castings. Work in 1963 was successful in adding the nodular graphite series chart to Method A 247. George A. Moore of the National Bureau of Standards made some very early quantitative measurements of these chart pictures using a computerized system developed at NBS. (Dr. Moore was an interesting person and Sub XIV meetings were never complacent events when he was present.)
Sub 14 has sponsored four symposia and published each, the last being held in May 1990 and dedicated to Dr. Halle Abrams, long time member and former Sub XIV chairman who died of a heart attack in October 1989. Halle had been involved in all four of E-4's MiCon (Microstructural Control) conferences. Sub XIV's initial efforts in quantitative metallography were in the domain of manual methods. Its first standard was E 562, Practice for Determining Volume Fraction by Systematic Manual Point Count. Manual methods have not been forgotten as automated methods have become popular. 33,34 Sub 14 wrote a standard practice for measuring decarburization, the original goal of Sub X when it first formed in 1949, and has a manual approach (which can be automated) for assessing banded or elongated microstructures. George Moore's efforts in the 1960s and 1970s to develop image analysis procedures for measuring structures, like inclusions, have been achieved in the last several years with three image analysis standards: E 1122, Practice for Obtaining JK Inclusion Ratings Using Automatic Image Analysis; E 1245, Practice for Determining Inclusion Content of Steel and Other Metals by Automatic Image Analysis; and E 1382, Test Methods for Determining the Average Grain Size Using Semiautomatic and Automatic Image Analysis. Practice E 1122 describes an image analysis approach for obtaining JK inclusion ratings according to methods A and D of Practice E 45, a manual chart method. It is presently being pursued aggressively by image analysis manufacturers and steelmakers. Practice E 1245 describes a stereological approach for measuring second-phase particles, such as inclusions, and it too is gaining interest in the market place. Practice E 1382 describes approaches for measuring grain size using semiautomatic and automatic image analyzers (WebMaster's note: see article) and has just been issued. With these three standards, Committee E-4 has been leading the way, pushing the development and use of image analyzers. Hence, they have been better than timely!
Sub 14 has several projects under way. A new task group was formed to explore evaluation procedures for thermally-sprayed coatings. Sub 14 is also trying to develop an image analysis procedure for assessing the shape of graphite in cast iron and is working on an approach to classify grain boundary carbide films in sensitized austenitic stainless steels. In the equipment area, Sub 14 is trying to develop a calibration test slide that could also be used to test out newly written computer measurement programs for precision and accuracy.
Sub XV on Emission Microscopy was formed in December 1968 with Dr. Erwin Eichen of Ford Motor Co. as chairman. This sub was to cover scanning microscopy while Sub XI would cover transmission microscopy. The work on the SEM resolution standard, Practice E 766, actually began under Sub XV, but was completed under Sub 11. Sub XV did hold a symposium, published as STP 485, Energy Dispersive X-Ray Analysis: X-Ray and Electron Probe Analysis. In 1977, Sub XV was merged back into Sub XI. Sub 16 on Phase Identification in Metal Alloys was established in November 1977 with Rick Anderson-Decina as chairman. The work on Practice E 963, reported above, was moved under Sub 16. In 1983, when Practice E 963 was issued, Sub 16 was merged into Sub 11.
Sub 17 on Laboratory Evaluation and Safety began as special subcommittee E04.94 on Standard Recommended Practice for Evaluation of Metallographic Laboratories on Nov. 14, 1977, under chairman Fran Warmuth of Special Metals Corp. (now with Cameron Forge Co.). At that time, ASTM was recommending that the 'E' committees create standards governing the evaluation of laboratories. In 1981, this group became Sub 17, the same year that it issued standard E 807 Practice for Metallo- graphic Laboratory Evaluation. Sub 17 is now revising Practice E 807 and is working on a guide to laboratory safety under Linda K. Kern of Kaiser Aluminum Co.
Committee E-4 has accomplished a great deal in its 75 years of voluntary service to the technical community. Those accomplishments have come from the dedicated efforts of many individuals, both well known and not so well known, but all working together. We need to remind ourselves regularly of our goals so that we can continue to build upon the shoulders of these giants of the past. There are stiII many worthwhile areas of endeavor for E-4 activity despite our past accomplishments.
1Groesbeck, E. C., "Solutions for Carbides, Etc., in Alloy Steels," ASTM Proceedings, Vol. 26, Part 1, 1926, pp. 569-571 and Vol. 27, Part 1, 1927, pp. 601-607.
2Wyman, L. L., "The Plastics for Mounting of Metallographic Samples," ASTM Proceedings, Vol. 38, Part 1, 1938, pp. 511-515.
3WyMan, L. L., "A Mid-Century of Metallography-Retospect and Aspect," Fifty Years of Progress in Metallographic Techniques, ASTM STP430,ASTM, Philadelphia, 1968, pp. 1-16.
4"What Can Be Done to Improve Alloy Phase Nomenclature?," ASTM Bulletin, December 1957, pp. 27-30.
5Fink, W. L., and Wyman, L. L., "The New ASTM System of Alloy Phase Nomenclature,"Materials Research & Standards, Vol. 1, April 1961, pp. 289-290.
6Rawdon, H. S., "Report of Sub-Committee V on Micro-Hardness," ASTM Proceedings, Vol. 26, Part 1, 1926, pp. 572-580.
7Vander Voort, G. F., "Results of an ASTM E-4 Round-Robin on the Precision and Bias of Measurements of Microindentation Hardness Impressions," Factors That Affect the Precision of Mechanical Tests, ASTM STP 1025, ASTM, Philadelphia, 1989, pp. 3-39.
8VanderVoort, G. F., "Operator Errors in the Measurement of Microindentation Hardness," Accreditation Practices for Inspections, Tests, and Laboratories, ASTM STP 1057, ASTM, Philadelphia, 1989, pp. 47-77.
9Mogerman, W. D., Zay jeffries, ASM, Metals Park, OH 1973.
10Bain, E. C., Pioneering in Steel Research, ASM, Metals Park, OH, 1975.
11McKeehan, L. W., "Glossary of Terms Relating to X-Ray Metallography,"ASTM Proceedings, Vol. 26, Part 1, 1926, pp. 582-589.
12 "Report of Subcommittee VI on X-Ray Metallography,"ASTM Proceedings, Vol. 25, Part 1, 1925, pp. 444-485.
13Moyer, R. B., "Committee E-7 on Nondestructive Testing: An Overview,"Standardization News, Vol. 10, Nov. 1982, pp. 12-13.
14"The Joint Committee on Powder Diffraction Standards- an International Data Resource," Standardization News, Vol. 2, July 1974, pp. 26-27.
15"Hanawalt, J. D., et al., "Chemical Analysis by X-Ray Diffraction," Ind. and Eng. Chem., Analytical Ed., Vol. 10, No. 9, September 15, 1938, pp. 457-512.
16Matthews, F. W., "A Coordinate Index to X-Ray Powder Diffraction Data Using Punched Cards," Materials Research & Standards, Vol. 1, August 1962, pp. 643-645.
17"New Retrieval System Developed for X-Ray Powder Data," Materials Research & Standards, Vol. 1, October 1962, pp. 842-843.
18McMurdie, H. F., "Progress in X-Ray Diffraction Data Compilations," Fifty Years of Progress in Metallographic Techniques, ASTM STP 430, ASTM, Philadelphia, 1968, pp. 192-200.
19Wyman, L. L., "The New ASTM Grain-Size Methods,"ASTM Bulletin, July 1956, pp. 59-61.
20Wyman, L. L. , and Penrod, R. E., "For a Unified Grain-Size Standard," Materials Research & Standards, Vol. 1, August 1961, pp. 638-639.
21Abrams, H., "Grain Size Measurement by the Intercept Method," Metallography, Vol. 4, February 1971, pp. 59-78.
22Davis, C. H., "Grain Size Comparator," ASTM Bulletin, August 1941, p. 45.
23Hull, F. C., "A New Method for Making Rapid and Accurate Estimates of Grain Size," Trans. AIME, Vol. 172, 1947, pp. 439-451.
24Morse, J. P., "Standard Methods for Characterizing Duplex Grain Sizes," Standardization News, Vol. 15, December 1987, pp. 44-46.
25Epstein, S., "A Suggested Method of Determining the Cleanness of a Heat of Steel," Metals and Alloys, Vol. 2, October 1931, pp. 186-191.
26G. W. Walker, "Rating of Inclusions ("Dirt Chart")," Metal Progress, Vol. 35, February 1939, pp. 169,170 and 167.
27"Detection of Inclusions in Bearing Quality Steel by the Ultrasonic Method,"Materials Research & Standards, Vol. 9, September 1969, pp. 21-24, 72.
28Donachie, M. J., Jr., and Kriege, O.H., "Phase Extraction and Analysis in Superalloys-Summary of Investigations by ASTM Committee E-4 Task Group l," Journal of Materials, Vol. 7, September 1972, pp. 269-278.
29Donachie, M. J., Jr., "Phase Extraction and Analysis of Superalloys-Second Summary of Investigations by ASTM Subcommittee E04.9l,"Journal of Testing and Evaluation, Vol. 6, May 1978, pp. 189-195.
30Chopra, K. S., "Interlaboratory Measurements of Amphibole and Chrysotile Fiber Concentration in Water,"Journal of Testing and Evaluation, Vol. 6, July 1978, pp. 241-247.
31 "E-4 to Review Calibration Practice for Scanning Electron Microscopes,"Standardization News, Vol. 8,July 1980, p.19.
32"SEM Performance Characterized," Standardization News, Vol. 13, February 1985, p.18.
33Abrams, H., "Quantitative Metallography,"Standardization News, Vol. 5, December 1977, pp. 16-18.
34Vander Voort, G. F., "Advances in Microstructural Imaging-Directions in Metallography,"Standardization News, Vol. 16, November 1988, pp. 50-57; and Vol. 17, February 1989, p. 12.