Herbert A. Laitinen Graduate Research Professol University of Florida Gainesvilie. Fla. 3261 1
Edward J. Meehan Professor Emeritus University of Minnesota Minneapolis, Minn. 55455
HAPPY BIRTHDAY I.M.~OL~OF
him up to that time is also included in that article. To sort out and describe the truly monumental scientific contributions of 68 years (now numbering 933 papers in addition to the books and monographs mentioned below) is indeed a formidable task. Of these publications, about 133 have appeared since Kolthoffs “retirement” in 1962. At least a dozen major research areas were interwoven with long overlapping periods among them. The common thread is the scientific approach to 248A
ANALYTICAL CHEMISTRY, VOL. 56, NO
9
FEBRUARY 1984
analysis, which is widely accepted today but which was rare in 1911, when Kolthoff entered the University of Utrecht. At that time, analytical chemistrv was essentiallv an emoirical art rathe; than a scientific discipline, and it was taught as such in most universities. By the fortunate accident of lacking courses in Latin and Greek, which were prerequisites to the study of the “pure” sciences, Kolthoff came under the tutelage of Professor Nicho0003-2700/84/0351-248A$0 1.50/0 0 1984 American Chemical Society
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HAPPY BIRTHDAY I.M. KOLTHOFF las Schoorl, who taught analytical chemistry and pharmacology in the School of Pharmacy at the University of Utrecht. Schoorl was highly skilled in analytical chemistry and deeply interested in a scientific approach to the subject. He was quick to recognize the exceptional talents of his student and encouraged him to carry out independent research a t an early age, pointing out promising directions and offering guidance, hut not intruding and rarely appearing as a coauthor. Another early influence was Kolthoffs acquisition in 1912 of a used copy of a book published by the noted physical chemist Wilhelm Ostwald in 1894, the year of Kolthoffs birth. This book, entitled “Die Wissenschaftlichen Grundlagen der Analytische Chemie” was later described by Kolthoff as the first scientific textbook in the field of analytical chemistry. The many marginal notes and comments in Dutch, German, and English attest to his thorough study of this hook.
Acid-Base Titrations, pH, Buffers, and indicators S.P.L. Sorensen had defined pH in 1909, Niels Bjerrum had carried out
fundamental work in acid-base reactions, and Leonor Michaelis had written monographs on hydrogen ion concentration and redox potentials by the time Kolthoff was ready to begin research, hut these studies were hardly known to analytical chemists of the time. Schoorl pointed out to Kolthoff a paper written hy Joel H. Hildebrand (2) in 1913 on acid-base titrations using the hydrogen electrode with a calomel reference electrode. Many years later, when Kolthoff was presented with the Nichols Medal, he referred in his talk to Hildehrand as one of his teachers. Hildebrand wrote him a nice letter in which he said, “You found gold where others found only dust.” In 1914, Schoorl had no equipment for potentiometric measurements, so each Saturday afternoon Kolthoff would carry his bottles of reagents to the laboratory of Professor Ringer in physiological chemistry. Ringer had precise equipment for pH measurements, hut he did not allow others to meddle with it. Soon Kolthoff devised his own potentiometric apparatus in Schoorl’s laboratory. The apparatus consisted of a meter stick and slidewire with a Lippmann capillary electrometer as a null detector due to the lack of a suitable galvanometer. The first paper, on the titration of phosphoric acid as a mono- and dibasic acid, appeared in 1915. There soon followed a succession of both fundamental and practical studies on acid-base behavior, ranging from salt effects on dissociation constants to the study of urine and stomach juices. A new set of buffer solutions was introduced, and fundamental work on acid-base indicators led to his first monograph on the subject in 1922. This hook went through several German editions and was translated by N. Howell Furman in 1926. In 1937, it appeared as “Acid-Base Indicators,” written with the collaboration of Charles Rosenblum. This pioneering work was not immediately accepted as valid analytical chemistry. Kolthoff has spoken of a colleague who referred to him disparagingly as “the pH-er” (or phonetically in Dutch the “pay-Haher”).
Redox and PrecipitationTitrations Kolthoffs PhD thesis, entitled “Fundamentals of Iodimetry,” was presented in 1918. It led to a series of 19 papers published in 1919-20, describing a comprehensive study of the reactions involved, including observations on reaction mechanisms, side re-
N . Howell Furman of Princeton University was Kolthoff’s personal friend as well as a professional colleague 2501
ANALYTICAL CHEMISTRY. VOL. 56. NO. 2. FEBRUARY 1984
actions, indicator function, sources of error, etc. Iodometric methods remained for years a favored area to which he returned time and again. Intermingled with conductometric and potentiometric studies were many classical titrimetric studies, culminating in 1927-28 with the publication of a famous book, “Massanalyse,” in two volumes. This book appeared in 1928 as “Volumetric Analysis,” coauthored and translated by N. Howell Furman. A three-volume version appeared later, coauthored by Vernon A. Stenger, George Matsuyama, and Ronald Belcher. In its several editions, this work has served for more than half a century as a reliable and critical reference work on classical analytical methods.
Conductometric Titrations Although conductance measurements had been made as early as 1875 hy Kohlrausch, and a few scattered papers by others had described primitive titrations based on conductance measurements, no one had studied them systematically for analytical purposes before Kolthoff began his research on this subject in 1918. He first published a paper entitled “The Importance of Electrical Conductivity in Analytical Chemistry” that year, followed by a series on acid-base and precipitation titrations. This work culminated in a monograph on the subject in 1923, entitled “Konductometrische Titrationen,” an early example of what would be classified today as an instrumental method of analysis. Incidentally, Kolthoff has never been fond of that term, prefer(continued on p . 254 A )
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HAPPY BIRTHDAY I.M.KOLTHOFF ring instead to speak of physical or physicochemical methods.
Potentiometric Titrations Kollhoffs entry into potentiometric measurements came through pH measurements, but as early as 1919 he had published a paper entitled “The Oxidation Potential of a Ferri-ferrocyanide Solution.” In that same year he puhlished a paper entitled “The Estimation of Ferrous Iron by Electrometrir Titration.” Ry 1920 he had introduced the termporenriomerric rirra[ions and had written a review paper on their applications. In 1924, Charles W. Foulk of Ohio State University, who had been work. ing in Ostwald’s laboratory, visited him in Utrecht and suggested a lecture tour in America. That same year Kolthoff made a historic visit. beginning with a meeting in Toronto and continuing with visits to Princeton, Ohio State. Illinois, Northwestern, and the University of Michigan. Most important were his first meetings with N. Howell Furman at Princeton and Hobart H. Willard at Michigan. Relationships among these three Americans and Kolthoff were always of personal friendship and deep mutual respect. All represented the scientific approach, and all had made early contributions to electroanalytical chemistry. Foulk had introduced the”dead. stop” endpoint, an early version of amperometric titrations: Willard (with
Florence Fenwick) had written significant papers on polarized electrode titrations; Furman had shown an early interest in potentiometric titrations. Furman made plans to spend a year in Holland with Kolthoff, but those plans were later changed because in 1927 Kolthoff accepted a professorship a t the University of Minnesota. Furman studied instead with W. D. Treadwell in Zurich, but with Kolthoff he coauthored the important book “Potentiometric Titrations,” published in 1926 and revised in 1931. This book has served for decades as the standard work in its field. Another American analytical chemist much admired by Kolthoff is Ernest H. Swift, whom he did not meet until many years later. In 1983, on the occasion of receiving the first ACS Analytical Division Award for Excellence in Teaching, Kolthoff remarked that if this award had been initiated 50 years ago, his chances of being the first recipient would have been “slightly less than 25%; naming these colleagues as worthy competitors.
Formation and Properties of Precipitates As an undergraduate, KolthofFs first gravimetric assignment was to determine sulfate as the barium salt. He said later, “I‘m not famous for having much patience. So I’m quite sure I didn’t wait every time when I washed the filter to make sure that all the water had gone through. I knew what the answer had to be, so I knew myself that I got a high value. 1 had to record it to be honest.” Professor Schoorl, apparently impressed by his honesty, referred his pupil to two papers he had written in the Journal of the American Chemical Society in
1912 on coprecipitation.
Another professor who was to have a profound and lasting influence on Kolthoffs career was H. Kruyt, the noted colloid chemist. Kolthoff had taken some courses from Kruyt and often sought him out for discussions. In 1915, pharmacy moved to a new building adjacent to the van’t Hoff laboratory (where Kruyt had an office) and connected to it by a corridor. Kruyt would use a signal-placing a book in his office window-to indicate, “OK, I’m not too busy. You can come.” Later, about 1926, when Kruyt was Baker Lecturer a t Cornell University, he was approached by S. C. Lind, head of chemistry a t Minnesota, for suggestions as to a strong research chemist to bolster the graduate research program. Kruyt recommended Kolthoff, who accepted a professorship in 1927. In 1920-21, Kolthoff published a series of nine papers on the significance of adsorption in analytical chemistry. This work languished for several years, except for a few papers describing adsorption on charcoal and the use of adsorption indicators in precipitation titrations, until 1932 when it was resumed a t Minnesota. A series of 38 papers on the formation and properties of precipitates was begun in 1932 and continued until 1947. What distinguished this series from most of the other work on classical analysis is that it was primarily directed to a general understanding of phenomena rather than to specific analytical methods. I t was puhlished largely in journals of general interest, such as the Journal of the American Chemical Society and the Journal of Physical Chemistry, rather than in analytical journals, which in that period were more recep-
Hobart Willard ( l e f t ) of the llniuersity of Michigan was a respected colleagup and friend of Kolthoff. Jaroslau Heyrousky (aboue) interested Kolthoffin polarosraphy 254A
ANALYTICAL CHEMISTRY. VOL. 56, NO. 2. FEBRUARY 1984
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tive to papers of immediate applicability. It is also noteworthy that quite a variety of experimental methods were involved. Tracer studies with radioactive isotopes, first thorium B as a naturally occurring isotope.of lead and later bromine activated by neutrons from a radon-beryllium source. were important. Surface area measurements were made by dye adsorption, monitored by a filter photometer.
Polarography and Amperometry In 1924, a Czech, Oldrich Tomicek, worked with Kolthoff for a year in Utrecht on potentiometric titrations. Tomicek later became a professor of analytical chemistry a t Charles University in Prague. Kolthoff visited Prague every two years, and had met Heyrovsky, the inventor of polarography, but did not become interested in that subject until 1933 when Heyrovsky visited Minnesota on a lecture tour. Kolthoff still speaks of “the famous week” when both Heyrovsky and Otto Hahn visited. Hahn was interested both in adsorption on precipitates and the use of radioactive tracers, which were active research areas at Minnesota. James J. Lingane had worked for several years as an undergraduate research assistant under Kolthoff and had coauthored about a dozen papers by the time he was beginning graduate work. Lingane built a manual apparatus and spent the next few years studying the fundamentals of the dropping mercury electrode. H. A. Laitinen began working on solid microelectrodes in 1936. Several other students entered the field soon, but not a single publication on the subject appeared from Minnesota until early 1939, when Kolthoff and Lingane published a 94-page paper in Chemical Reviews. A number of US.lahoratories had purchased recording polarographs manufactured in Prague, but the publications were few in number and largely empirical in nature. The appearance in 1941 of the first edition of the monograph “Polarography,” coauthored by Kolthoff and Lingane. was a great stimulus to the scientific development of the polarographic method, especially in the U S . Much of the early fundamental work of the Czech school had escaped the attention of American analytical chemists, and the onset of World War I1 in 1938 interrupted communications as well as many research programs. Although the Czechs had performed titrations using the dropping mercury electrode, Kolthoff did not like their designation, polarometric titrations, and in a paper with Y. D. Pan in 1939 he introduced the name amperometric titrations. The term voltammetry was
HAPPY BIRTHDN I.M. KOLLTHOFF
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first used in a paper with H. A. Laitinen in 1940. Kolthoff has credited Nernst with the introduction of both of these methods in a primitive form early in the 20th century. Fruition of these methods was to come from the work of others, but Kolthoffs work provided an important stimulus. After about 1950, profound changes occurred in microelectrode studies. both because of the introduction of modern electronic instrumentation and the interpretation ofcurrenttime-potential relationships through modern theory. Although Kolthoff himself has never professed a deep in. terest in electronics or instrumenmtion. it is significant that the several generations of his former students and associates have made their share of the modern developmenm.
Emulsion Polymerization Early in World War II the U.S. was cut off from its supply of natural rubber, and the existing production of synthetic rubber was far too small to supply the urgent wartime needs. The government established a comprehensive research and development program for the production of synthetic rubber, using the existing CR-S (government ruhher-synthetic) recipe. A t that time the kinetics and mechanism of the complicated reaction were practically unknown. The major rubber companies cooperated in the program, and several eminent university professors were asked to participate. Among
these were physical chemist P. Debye, organic chemists C. S. Marvel and M. Kharasch, colloid chemists W. D. Harkins and J. W. McBain, and analytical chemist Kolthoff. Kolthoff was asked to develop analytical methods for the various constituents so that the rate at which they were consumed during reaction could he determined. One constituent, n-dodecyl mercaptan, was referred to as “OEI,” standing for “one essential ingredient.” In its absence practically no polymerization occurred, and with either too much or too little the physical properties of the product were unsatisfactory. A major difficulty in large-scale production was that the properties of the polymer frequently were irreproducible; this was presumed to be due to irreproducible consumption of the mercaptan. Kolthoff quickly developed a simple and accurate method for the determination of this and other mercaptans by amperometric titration with silver nitrate. This method is used worldwide today. The paper describing the method, which appeared in 1946, was described by Current Contents (July 7,1980, p. 10) as “This Week‘s Citation Classic”; it was cited over 130 times between 1946 and July 1980. Not content simply to develop methods, Kolthoff characteristically undertook with W. E. Harris a comprehensive investigation of the factors affecting the rate of reaction of this and other mercaptans and established that the kind and intensity of agitation during reaction are of decisive importance. Largely as a result of these studies it became possible to recommend proper agitation for largescale reactors and to avoid wasteful overconsumption of what was then a chemical in very short supply. Kolthoff also developed methods, too numerous to list here, for other constituents. Mention should be made, however, of the simple and accurate method be and Harris developed for gel content of the polymer, which likewise is still in use. Other work included a comprehensive study of the entire kinetics and mechanism of emulsion polymerization, including the role of soap and detergents, and of persulfate and other initiators. This led ultimately to the development of new initiating systems which permitted practical polymorizations a t temperatures much lower than 50 “C, at which the original G R S reaction took place. The lowtemperature rubbers proved to have superior properties. Again characteristically, Kolthoff brought out a comprehensive monograph on the subject coauthored by his collaborators F. A. Bovey, A. 1. Medalia, and E. J. Meehan.
AN4LYTICAL CHEMISTRY. VOL. 56. NO. 2. FEBRUARY 1984
257A
Kinetic Methods of Analysis In the work on emulsion polymerization referred to above, one of the major early problems concerned the structure of the copolymer of butadiene and styrene. It had long been recognized that (among other possibilities) a butadiene molecule could add to a free radical in 1.2 or 1,4addition. The former process leads to a side chain, the latter to a linear adduct, giving rise to an external and internal carbonxarbon double bond, respectively. Studies with T. S. Lee of the rate of addition of iodine monochloride to unsaturated compounds showed that this substance adds to external and internal bonds a t different rates. This led to a kinetic method for determining the relative amounts of the two kinds of bonds. While nowadays an IR method is quicker than the kinetic method, it should not be forgotten that the IR method is not absolute and must be calibrated by the kinetic method. Induced Reactions Long ago it was known that the reaction between iron(1I) and permanganate induces the reaction between hydrochloric acid and permanganate. Many similar examples are known in both organic and inorganic chemistry. Kolthoff‘s work with A. I. Medalia established the details of the reaction between iron(II) and hydrogen peroxide. Hydroxyl radicals are formed in the first step of this reaction. Under some experimental conditions, these radicals can lead to pronounced deviations from the expected simple reaction ratio (21).Perhaps of greater significance is the fact that in the presence of many organic compounds the hydroxyl radicals can bring about the induced oxidation of the organic compound. The iron(I1)-peroxide reaction has long been used in organic synthesis (Fenton reaction), but we owe our detailed understanding to Kolthoff and Medalia. Among other studies on induced reactions, too numerous to be listed here, mention should be made of the study with R. W. Woods, which established the complicated details of the oxidation of arsenic(II1) induced by the reaction between iron(l1) and persulfate and catalyzed by copper(1I).
Nonaqueous Solvents Nonaqueous solvents have long been of interest to Kolthoff, going back to his very early work on acidbase behavior in methanol and ethanol. The work with S. Bruckenstein on glacial acetic acid is of particular interest. When the work was begun, there was already a considerable amount of empirical information about this solvent. It was known that 258).
HAPPY BIFUHDAY I.M. KOLTHOFF
Kolthoff in 1983upon receipt of the A C S Diuision ofAno/ytico/ Chemistry Award for Excellence i n
Teaching
no substance was fully dissociated in acetic acid. No interpretation could be given to acid-base titration curves, which in some instances resembled that of a strong acid-strong base in water. Kolthoff and Bruckenstein were able to account quantitatively for these and many other experimental observations. In later years, M. Chantooni has collaborated with Kolthoff in fundamental studies of other solvents, including acetonitrile and dimethylsulfoxide. As the dielectric constant of the solvent decreases, the quantitative interpretation of the titration data becomes increasingly complicated. In the case of the weak acid HA, for example, it is necessary to take into account a reaction such as A-
+ HA = HA?-
or even the formation of A(HA).-. Because such equilibria are concentration dependent, the interpretation of conductometric titrations, for example, is somewhat involved. We are indebted to Kolthoff and Chantooni for a splendid chapter on acid-base reactions in nonaqueous solvents in the second edition of the Kolthoff-Elving treatise (Part 1, Vol. 2).
Macrocyclic Ligands As soon as J. Pedersen published his paper in 1967 on what are now called crown ethers, Kolthoff realized the tremendous analytical potential of
ANALYTICAL CHEMISTRY, VOL. 56. NO. 2, FEBRUARY 1984
such compounds and began a study with M. Chantooni which still continues. This led, in addition to the expected new and valuable methods, to the comprehensive review in ANALYTICAL CHEMISTRY(1979,51,1R).The review contains 207 references and this statement, which all reviewers should take to heart: “The publications referred to in the present paper have all been read by the author.” The author concludes with the characteristic statement: “This review has been written to stimulate more research on the analytical applications of macrocyclic ligands.” It then goes on to list 13specific problems which deserve further study.
Books “Treatise on Analytical Chemistry.” This monumental treatise, edited by Kolthoff and Philip J. Elving, is a unique contribution. As all analytical chemists must know, i t is in three parts. The first, “Theory and Practice,” is devoted to basic fundamentals and general principles. It consists of 11 volumes (7232pp.) plus an index volume, and appeared over the period 1959-76. Its success was so great that a second, much enlarged edition is in progress, and as of this writing eight volumes have appeared. The second part, “Analytical Chemistry of Inorganic and Organic Compounds,” consists of 16 volumes (8054pp.) plus an index volume, and appeared over the period 1961-80.The third part, “Analytical Chemistry in Industry,” is still in progress; four volumes have appeared so far. Examination of the treatise in any library readily shows the amount of use it receives. Textbooks. Several of the monographs mentioned above have seen extensive use as reference works and textbooks in the classroom. T h e book “pH and Electrotitrations” was written expressly as a text for an advanced undergraduate-first year graduate course taught for many years by Kolthoff. A second edition, enlarged to include amperometric titrations, was coauthored with H. A. Laitinen and appeared in 1941. The famous “Textbook of Quantitative Inorganic Analysis” was written with E. B. Sandell in 1936.After two more editions, a fourth edition with the new title “Quantitative Chemical Analysis” appeared in 1969,with Sandell, E. J. Meehan, and S. Bruckenstein as coauthors. In 1936 this was perhaps the first analytical text to combine a thorough treatment of the fundamentals with a wealth of practical material. Moreover, what was rare at the time, it contained many references to the original literature. The continued worldwide success of this text is shown by the fact that the (continued on p. 262 A )
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granted. For added convenience, an alphabetical index of faculty members is included. The 1983 Directory lists information that is current as of the 1983-84 academic year and includes 715 departments, 9,285 faculty members, and 57,833 publication citations. The cost for this hard cover, 1231-page volume is $43.00. To order a copy, Call Toll Free 1-800-424-6747 or mail the coupon below. Special Note:The entire 1983 Directory, including a concordance of the research interests of each faculty member listed in the Directory, will soon be available as an on-line computer-readable file. Write to the ACS Office of Professional Training, 1155 16th Street, N.W., Washington, D.C. 20036, for further details.
American Chemical Society, Department 706, P.O. Box 57136, West End Station, Washington, DC 20037 Please send ___ copies of the 1983 ACS Dlrectoryof GraduateResearch@ $43 per copy. On prepaid orders (including credit card orders) ACS pays shipping and handling charges. On purchase orders, shipping and handling fees will be added. For single orders of 20 or more copies, a 5% discount is available.
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HAPPY BIRTHDAY I.M.KOLTHOFF fourth edition has been translated into Italian, Japanese, and Spanish.
Scientific Progeny In the long run perhaps the most important contribution to science of someone like Kolthoff is the lasting and growing influence on several generations of students. It is no easy task to trace this lineage, because consideration must be given not only to the direct line from professor to PhD student hut to several less direct types of influence as well. In the direct line, one can trace numerous examples of four scientific generations, e.g., Lingane-Bard-Faulkner-students; or Hume-Purdy-Christian-students; or lait inen-Enke-Nieman-students;
and a few examples of five generations. Through 1982, Kolthoff has produced close to 1100 PhD "offspring." However, there are many examples of ex-students teaching in non-PhDgranting institutions who are sending BS and MS chemists on to other schools for further study. A good example is the line Sandell-Ramettestudents. Of course, many BS and MS chemists are also educated in PhDgranting departments, and the lines of scientific influence can become greatly entangled. An example is the Laitinen-Holtzclaw-Collman line. James Collman received his MS degree under Holtzclaw as an inorganic major, hut went on to graduate work in the field of organic chemistry and is now a professor in that area at Stanford. Another type of entanglement is encountered with the many postdoctoral students of Kolthoff. It would not be proper to claim many of these as direct progeny, especially if they came as mature scientists for just a year or two of study and then returned to their permanent positions. However, there are some exceptions, in which the postdoctoral influence proved to be a turning point, such as Joseph Jordan who went on to an academic career in areas initiated during his postdoctoral study. Less direct influences are those exerted by ex-students on their colleagues and on students of other professors through undergraduate and graduate courses. Such influences are more subtle hut no less real than the direct ones. In the same vein are the influences exerted in industrial laboratories by research managers on younger chemists. A few examples are represented by Vernon Stenger (first 262 A
-
generation) and Warren Crummett (second generation) a t Dow, the late Henry Yutzy a t Eastman Kodak, and Frank Bovey a t Bell Laboratories.
Conclusion In this htief account of the scientific accomplishments of Izaak Maurits Kolthoff, we have concentrated on just one aspect of a long and wellrounded life. We have omitted mention of his efforts on the political scene to foster international understanding, on the social scene to rescue scientific colleagues from oppressive regimes, his interests in cultural events, his athletic interests, his courageous battles with various physical setbacks, and his vigorous and stimulating interaction with students and colleagues. We leave to future historians the formidable and rewarding task of recounting these matters. References (1) Lingane. James J. Talanta
1964.11,
67-73.
(2) Hildehrand, Joel H. J . Am. Chem. Sac. 1913.3% 847.
Herbert A. 1.aitinr.n rcwit,rd his PhD from the Uniwrsily f ~ fMinnesota in 1940. In that year, he joined the faculty at the Uniuersity of Illinois where he remained until 1974 when he assumed his present position as graduate research professor at the Uniuersity of Florida. Professor Laitinen was the Editor o f ANALYTICAL CHEMISTRYfrom 1966-79.
Edward J . Meehan rrcriued his BS degree in 1933 and his PhD in 1936 from the Uniuersity of California, Berkeley. He remained at Berkeley as an instructor until he moued to Minnesota in 1939. In 1982 he retired as professor emeritus o f analytical chemistry.
ANALYTICAL CHEMISTRY, VOL. 56. NO. 2. FEBRUARY 1984
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