FILE: C:\User-Nathan\Data\WP Documents\NateBio Part II Chapter VII.wpd
Chapter VII Purdue University: September 1947 through January 1951
Purdue University is located in West Lafayette, Indiana, 65 miles northwest of Indianapolis and 126 miles southeast of Chicago. Lafayette and West Lafayette are separated by the Wabash River. The twin cities are located in Tippecanoe County. The name, Tippecanoe, commemorates the 1811 Battle of Tippecanoe in which William Henry Harrison, later the ninth president of the United States, decisively defeated the forces of Indian Chief Tecumseh.
From the time I left New York City to travel to West Lafayette, Indiana, and the time that Galla arrived about a month after I got there, it is difficult to record the chronological sequence of events because of memory lapses. It must have been the at beginning of September that I boarded a train for the overnight ride to Lafayette, Indiana. I don’t believe that there was a direct route to Lafayette; I must have changed trains in some city, but where I did this is forgotten. I arrived in Lafayette sometime in the morning. I must have been carrying a suitcase, but I have no recollection of what I did with it as I headed for the Purdue University campus. I probably used a local bus to take me to West Lafayette and I probably got off the bus at the Purdue Memorial Union Building. .
The Purdue Memorial Union is north of West State Street and west of the corner at Grant Street. The Memorial Union is a center of activity for students, staff, and visitors. In the Memorial Union building there was a cafeteria, rooms for visitors to stay in while on the campus, and offices for various student activities. After a short walk to the Chemistry Building, which is a bit north and west of the Memorial Union, I headed for the Chemistry Department office.
My first priority was to found some housing. I was told that because of the great influx or returning veterans to the campus housing was at a premium. I was directed to an office which arranged for student housing. I was told that there were apartments for graduate students in brick buildings on the north side of the campus but they were all taken, some by faculty members. There were apartments in converted army barracks near the Purdue University Airport, however they were for students with families. In essence, I was told that I had to go hunting elsewhere. I went back to the Chemistry Department and complained about the treatment at the housing office. I had the chutzpah to say that I would go back to New York if I could not be placed in a student housing project. I guessed right; there was a dire need for teaching assistants. The Chemistry Department intervened for me and I was assigned an apartment in one of the barracks buildings. The address for us would be 543-3 Airport Road, West Lafayette, Indiana.
I suppose that after being assigned an apartment, I must have taken a local bus which had the University airport as its destination. After a short ride going west along West State Street, the bus turned south on Airport Road. When I got off the bus, I walked among a large complex of former army barracks that had apartments in them. The size of each building was 20 X 100 ft. There were four apartments with the address 543 and the -3 connoted the third apartment from north end of the building. The size of each apartment was about 500 sq. ft. The rent for the apartment was $30.00 per month. There were two side-by-side windows to the left of the entry and to the right of the entry. To enter the apartment, there was a step up to a wooden platform . There were two posts holding up a flat roof over the platform. I entered the apartment. There was a wall between the front and back of the apartment on my right. The sides of a small, no-door-closet extended into the room at the entry. At a short distance from the closet here was a door which led into the bedroom. On my entry into the bedroom, I found that there was a wall on the left which separated the bedroom of our apartment from the bedroom of the apartment with the address 543-4. The living room was on the left and there was a small kitchen behind the living room on the left. The kitchen was furnished with a gas stove and an ice box. There was a window in the kitchen from which one could look out at a lawn separating another building like ours. There was a gas stove along a short wall in back of the living room for heating the apartment. On looking out of the living room windows I could see the lawn dividing us from a similar building. There was a hallway opposite the entry door and in this hallway there was a door to a small bathroom on the left (back-to-back with the kitchen). A water heater was part of the furnishings. Te floor consisted of dark linoleum tiles.
I shopped at Sears Roebuck in Lafayette to buy a refrigerator and a Hollywood bed. This bed consisted of a mattress and a box-spring that had legs attached to it. Those items were delivered several days after the purchase. I know that I moved into the apartment quickly, but I have no recollection of my life in the apartment. I did meet several veterans who were also graduate students in the Chemistry Department and who with their families lived in the apartments on Airport Road. I know that I missed Galla and I called her quite often. I also know that I had no telephone in the apartment, so where I called Galla from is a mystery to me. I have a fleeting recollection of meeting Galla at the train depot in Lafayette about a month after I got there. Until Galla came I was kept busy with my introduction to the graduate school requirements, courses, and teaching assistant duties.
Although I came to Purdue University Graduate School Chemistry Department with a MA in chemistry from Columbia University, all it was good for is to provide 45 credit hours of chemistry courses. To meet the requirements for the Ph.D. degree, it was if I did not have the advanced degree. I had to take an examination to test my knowledge of written English usage. This test had to be taken before any plan of study could be approved. I was startled to learn that before I could take courses in The Chemistry Department, I had to take written tests which covered the four major fields of inorganic, analytical, organic, and physical chemistry. The requirements then called for 24 credit hours in a major, and 12 credit hours in each of two minor subjects. I selected organic chemistry as my major and analytical and physical chemistry as my minors. Looking back, I would have better off taking biochemistry as one of my minors. Then to start my required research project, I had to pass qualifying examinations in the four fields of chemistry as for the introductory tests. Once I passed the qualifying examinations I could start my research project and keep taking the necessary chemistry courses. When I felt ready, it was required that I take preliminary comprehensive written examinations for the major and minor subjects. At the time of these examinations, a committee of my major research advisor and faculty members representing the minor subjects was appointed. Upon passing all of the written examinations, I had to appear in front of the committee for an oral examination. I would only become a candidate for the Ph.D. degree not only by passing all the previous examinations but by passing the requirement of a reading knowledge of two foreign languages. The final examination would be when I would sum up my research results in a written thesis and appear in front of my committee to defend my thesis. .
I must have taken and passed the English test without any difficulty; it certainly left no lasting impression. But what has been a lasting impression has been the four tests that I took several days after arriving at Purdue University. The tests were given in the Chemistry Building auditorium on the street level floor. Dr. Henry B. Hass, the head of the Chemistry Department and Professor of Organic Chemistry, was standing in back of the long laboratory bench at the front of the auditorium. Our applications for admission to the graduate school, which had photos of the applicants, were lying on the bench top. Dr. Hass was the proctor for the four examinations. The tests were ones devised by the American Chemical Society. After I finished taking the last test, which was late in the afternoon, I was impressed when I realized that Dr. Hass knew each one of us by sight and name. I passed three of the tests with good grades, but I did not do well on the analytical chemistry examination. After all, the quantitative analysis course that I took at the university of California during the summer had not really prepared me for intensive testing in this subject. Not doing well meant that I had to take a remedial course.
The courses which I took during my first semester at Purdue University, the Fall 1947 semester, were Chem 151 Intermediate Analytical Chemistry, Chem 263 Advanced Organic Chemistry, and Chem 201C Organic Techniques.
I suppose that I did make contact with Dr. Philip Elving when I arrived at Purdue University as he was the one who arranged for my teaching assistantship offer. It was Dr. Elving who presented the intermediate Analytical chemistry course. Dr. Elving was an excellent teacher who made the quantitative analysis course far more informative than the course that I took during the summer of 1938 at the university of California. The textbook we used in this course was Textbook of Quantitative Inorganic Analysis, by I.M. Kolthoff and E.B. Sandell.
The advanced organic chemistry course was presented by Dr. Henry Hass. The over 1000 page textbook in this course was Organic Chemistry, by Frank C. Whitmore. The course consisted of three one-hour lectures periods a week. The standing assignment was that we were responsible for learning, actually memorizing, the organic chemical reactions presented in 10 pages of the textbook per lecture period.. Dr. Hass would call students by name to test their knowledge or the contents of the 10 pages assigned for that lecture period. We soon found out that Dr. Hass had a system where no student escaped from being called upon to answer a question. We had to be prepared. Dr. Hass would update any information in each of the 10 pages, if there was more current information.
The list of chemistry courses in the graduate school catalog included required technic courses. During this semester I enrolled in an organic technics course. I took it as a two credit course which meant two laboratory periods a week. There also was a one hour lecture period. The instructor for this course was Professor of Organic Chemistry Earl McBee. A textbook used in this course was Physical Methods of Chemistry, volume 1, Physical Methods of Organic Chemistry, edited by Arnold Weissberger et al. There were other volumes in this series and they served as reference books during my career as a chemist. The laboratory exercises were so designed that I had the opportunity to actually use technics which I had only previously.read about. The assigned laboratory exercises kept me working in the laboratory not only during the assigned hours but some evenings as well.
Beside taking three courses, I had teaching assistant duties. I was assigned to work under the direction of Frank Martin, Ph.D., Professor of General Chemistry. I was assigned to supervise the performance of laboratory exercises by a group of students in a general chemistry laboratory and I graded test papers. Dr. Martin had an interesting system of grading as the number 13 was used as a basic grade number rather than 10. Then at the end of the semester there was a mathematical formula into which a student’s grade was inserted to arrive at a final grade.
Although teaching assistants were supposed to attend the lectures given by Dr. Martin, the pressure of course work and getting settled at home prevented me from doing so constantly. Dr. Martin was a very good instructor and also one can say quite colorful. The lecture hall was one where at the front of the room there was a blackboard and a long laboratory bench, on a platform, perhaps about 12 inches high. The entrance to the room consisted of two doors at the front of the room. Tiers of seats were on a floor that sloped upward. Being that the entry doors were at the front of the room, Dr. Martin would be aware of anyone that came into the room while he was lecturing. Late comers were requested to be seated at the front of the room and these students were used to conduct the experiments that were being demonstrated. As an example, at one lecture, which has remained in my memory, is the demonstration of the generation of the gas hydrogen. One of the late comers was asked to some to the front of the room and place a lit match at the end of a tube through which hydrogen was emitted. Hydrogen can be explosive and Dr. Martin made some remarks which obviously scared the student. After the student finally applied a lit match the released hydrogen burned and there was no explosion. Then another unlucky student was called to the front of the room to activate a situation in which there was a controlled explosion. I doubt that these students or most the others ever came late again.
It was announced that if a teaching assistant did not attend Dr. Martin’s lecture a day before the Thanksgiving holiday, there would be a penalty. I came down with a bad cold that week and on the evening and day before Thanksgiving I had a fever, so I missed the lecture. On the morning of Thanksgiving Day there was a knock on our door and Dr. Martin was standing there. Galla invited him in and he saw me in bed. After a quick look, Dr. Martin brought one of his arms from behind his back and presented us with a bag of oranges. He thought that would be helpful in combating this respiratory infection.
I decided to take the written qualifying examinations at the end of the semester. If I passed them I could start my thesis research project. Three hours were allotted for each of the tests in the fields of inorganic, analytical, organic, and physical chemistry. Copies of former tests were available to the students taking the qualifying examinations, however, no one knew what to expect for the inorganic chemistry test. Dr. Herbert Brown, a future Nobel Prize winner had just joined the faculty of the Chemistry Department and he was the one responsible for the contents of the test. To my delight, I passed the qualifying examination s requirement and I could start on my Ph.D. research the next semester.
Being busy with course work and my teaching assistant duties helped pass the time until Galla joined me about a month after I arrived in West Lafayette. I know that I was living in our apartment where I had a bed and a refrigerator. I met neighbors and their families before Galla came. However, I also remember the sense of loneliness at the end of the day when I entered our living quarters. I had to use the local bus to travel between the university and our apartment. As the apartments were near the Purdue University Airport, however, we were isolated from shopping facilities. We had to travel by bus to shop for groceries in West Lafayette and for anything else we usually had to ride to Lafayette.
After I met Galla at the Lafayette railroad station, life became a bit easier. Galla had packed and shipped our personal belongings from New York City. Making the relatively empty apartment into a comfortable home was accomplished during our first year in residence. Russell Wright dishes of simple contemporary design were the rage among young newly-weds; we had purchased settings in greenish-blue color and light gray colors. We had been given a set of silverware by Galla’s parents for a wedding gift, however for every day use we bought stainless steel dinnerware. Galla had received a going away gift from fellow workers at the New York City Health Department on 125 Worth Street, Manhattan. This gift was a Silex glass drip coffee making set. Galla was and is not a coffee drinker, so this gift was used for guests only. I was a coffee drinker, so we purchased a one or two cup coffee-maker for my use. The items described above were packed and shipped. With other household items we began to make the apartment livable. We purchased a three sectional couch; two sections were placed against the window wall of the living room and one section was placed to the left of the entry door and facing the left wall of our apartment. We purchased a card table and four folding chairs. For our bedroom we bought several unpainted chests of drawers that we put a clear finish on ourselves. I am not sure if we purchased a kitchen table and two chairs or if we rented them from the university housing group. Somewhere in time we bought a small hand-powered device for washing and wringing laundry. I believe that we had a rope line for hanging wet laundry in back of our apartment. We purchased drapes for the windows and the open closet at the entry
Although I did not have good woodworking skills, it was Galla’s father, Monroe, who taught me how to make simple cabinets and bookcases We had a lumber yard cut out wood to our specifications and I used a hammer and nails to put together some cabinets and bookcases. Dark green paint for the bookcases and the outsides of the cabinets covered the raw wood. The cabinet doors were pained with gray paint and large square handles were pained dark green. I also made a corner table and I used some glass blocks for this item. Dark green paint was also used for the table.
We have no records of our financial status at this time. Part of my army pay was sent home where it was deposited in a bank account. Galla also had saved money attained from her job as a statistician with the New York City Health Department. After we were married, we placed our money into one bank account. I had subsistence money coming in from the G.I. Bill of Rights and there was some a modest income from my teaching assistantship. I suspect that our net worth was not very great.
We also had some social life with other graduate students. We had some student friends over for dinner. We played bridge with some graduate students and their wives. Later on we played bridge with faculty members in the Memorial Union building. The one football game that we went to see was during this semester when Purdue University played against Notre Dame and lost. There were two big football games for Purdue each season and they were with Notre Dame and the University of Indiana.
I registered for the following courses for the winter of 1948 semester: Chem 251, Current Techniques of Analytical Chemistry, Chem 299, Research in Chemistry, and Chem 264, Advanced Organic Chemistry. The advanced organic chemistry course was the second part of the course taken with Dr. Henry Hass during the Fall 1947 semester. Of course, I also had teaching assistant duties.
Now that I was able to start working on the research project for the Ph.D. degree, I conferred with Dr. Elving. At the southeast corner entrance to the Chemistry Building, at the top of the stairway on the first floor, on the immediate left, there was an entrance to an anteroom in back of which there was an entry into Dr. Elving’s office. On entering the anteroom, to the left, there was the entry into a laboratory. My first assignment of a research project was to produce polarographic data for a series of organic nitro compounds in aqueous solution. I was assigned the Sargent-Heyrovsky photographic recording polarograph. Two other graduate students worked in this laboratory under the guidance of Dr. Elving. One was Norman A., who came back from an absence to finish working on his thesis and the other was Charles T., who was doing a polarographic research project and then would do another project with Associate Professor of Organic Chemistry Nathan Kornblum, Ph.D. Charles T. was assigned a Leeds and Northrup polarograph, the Electrochemograph. We all pitched in to clean up this laboratory which had not been used for quite a while. In back of a top shelf of a wall mounted cabinet we found a standard Weston cell reference electrochemical cell. The voltage of this cell was on an attached tag and it was also stated that this voltage had been measured at the National Bureau of Standards in 1929. After our laboratory was set up we measured the voltage and to our amazement if corresponded to that of 19 years ago. Because of money from a grant, we had new and adequate equipment which made it possible to start work on our research problems.
About midway into the semester, I awoke one night after a nightmare and I was nauseated. We were scared as I felt ill with no apparent reason. Apparently there was a telephone outside of our apartment, so Galla called a physician. These still were days when physicians made house calls. After an examination, the physician suggested that we should come to his office during the day. No physical problem was found. However, I did not feel well for a while, so I took some leave and we went to New York City where we stayed with Galla’s parents in their house in Staten Island. Galla still belonged to the health insurance program HIP. I was examined at a New York University medical clinic and it was suggested that I had an anxiety problem from the pressure in graduate school. We returned to West Lafayette and I had some sessions with a clinical psychologist in the Psychology Department. Some insight developed about my anxiety state. The tensions from serving in a combat zone during the war which had not been released psychologically, the pressures of graduate school requirements, the pressure to succeed, the responsibilities of marriage, and the inability to take things as they were all clashed. There was a period of time in which I was not very productive in respect to my research problem.
I had to drop the teaching assistantship and I took incomplete grades in my courses. We now depended on an income from the G.I. Bill of Rights. Galla was able to find a part-time job in the statistics department.
For transportation between the apartment and the university or shopping facilities, we depended upon the local bus company. The winters in Indiana were usually very cold, windy at times, and often icey conditions prevailed. After standing and waiting for a bus under the usual weather conditions led me to the conclusion that we needed a car for transportation. It was difficult to buy a car in 1948 as the change-over from war to civilian production was low. One had to place a name on a list at a car dealer and then one had to wait for their turn to purchase a car. A war veteran who did have a car because he had a high priority in that he was quite disabled put his car on sale. Galla was angry because I just about offered all the money we had in the bank for the car and we were lucky in that the offer was not accepted. It was a very large graduate student who came from Texas and a very large dog began to be seen in a small car, the Crosley.
The Crosley became available for about $600. It had about an 80 inch wheelbase and the car itself was about145 inches long. The weight was about 1,150 pounds. The engine block was made of aluminum. We purchased a Crosley two-door pick-up or station wagon. As neither had a driver’s license Norman A, a laboratory partner, drove the car until we became licensed drivers. We were able to get an instructor to teach Galla how to drive. One had to use a cluth and shift gears on this car and for the shift to work well, we had to press down on thew clutch pedal to shift from neutral to first gear and then to press down on the clutch again to shift the gears from first to neutral to the usual gear used for normal driving (double-clutching). I had driven a Jeep (without a license , while overseas) and Galla’s mother taught me to drive their family car. After getting our driver licences we practiced driving in- and out- of town. We eventually began driving to Indianapolis for a buffet lunch at one of the hotels and some shopping. During the summer vacation we actually drove to New York City. I often say that when we came to a tunnel on the Pennsylvania Turnpike and saw a speed limit of 35 miles per hour speed limit, I had to jam down the accelerator to attain that speed. We had to shift to a lower gear for enough power to drive uphill on parts of our route to New York City. In New York City we stayed with Galla’s parents in their house in Fort Wadsworth, Staten Island. We visited my father and Mary on their farm. Norman and Norma were married December 22, 1947 and I believe they were living in an apartment in the Bronx when we visited them. I believe Norman was in the process of fnishing his work toward the Ph.D. degree at the Columbia University medical school biochemistry department.
The Crosley lasted about a year before the engine failed. The Crosley people redesigned the car with a cast iron engine block and we were able to change cars for $100. We took a bus to Marion, Indiana, where we picked-up a sedan at the factory. We were able to see the assembly line and we learned that this car was held together with nuts and bolts.
During the summer session of 1948 I registered only for the course Chem 299 Research in Chem. The courses I took during the fall semester of 1948 were, Chem 201A Glass Working, Chem 299 Research in Chem, Chem 291 Organic Reactions, and Chem 285 Advanced Physical Chemistry.
The glass working course was taught by Thomas DeVries, Ph.D., Professor of Physical Chemistry. In this course we were assigned simple items made of glass and gradually worked up to more complicated glass devices. Toward the end of the semester, Galla kept me company one evening when I worked to complete a glass working assignment. There was another graduate student also working on a glass working assignment. We chatted and during our conversation I mentioned that I had an M.A. from Columbia University. The student then asked, “Isn’t Columbia University a hotbed for communists?” Galla replied,”How many communists does it take to make a hotbed?” Our chatting ended.
I am unable to identify the instructor and the content of the organic reactions course. I suspect that the advanced physical chemistry course was given by Dr. Newton and it covered the phase rule. I had pleasant chats with Dr. Newton and I was sorry to see him leave Purdue University. Dr. Newton went on to work for Westinghouse in the Pittsburgh area.
Even though smoking is addictive, I was able to stop doing so at the beginning of the year just when iI felt that I need this outlet for the stresses and strains of attaining the Ph.D. degree. My father was a smoker and I tried to smoke during my last year in high school in order to show I was an adult. I did not become addicted and I stopped smoking quickly. I tried again during my senior year at the University of California and again I quit quickly. It was when I was inducted into the army that I started smoking again and this time I did become addicted. Cigarettes were free overseas and that did not help one stop smoking. By this time I was smoking cigars and pipes occasionally. It was in an organic chemistry course that I learned that some cigarette brands tobacco was wetted with ethylene glycol and in the body the ethylene glycol would be oxidized form oxalates, a basis for kidney stones. Furthermore, I began to have coughing spells. Quitting was difficult, but I managed to do so, and today I certainly have no regrets. However, it took a long period of time to lose that desire to reach for a cigarette.
I believe it was in February of 1949 that I registered for the following courses: Chem 264 Advanced Organic Chemistry, Chem 299 Research in Chem, and Chem 278 Electrochemistry.
Dr. DeVries was the electrochemistry instructor and he was not a very good lecturer. However, I found that on one on one meeting in his office, Dr. DeVries was able to explain concepts clearly; I do not understand why he couldn’t do so with his lectures. I did not do well in this course, however, I took the course again and I was able to get a good grade the second time.
The organic chemistry course was the second half of the one given by Dr. Hass and it had the same format as the first half of the course. My incomplete 1948 in Chem 251 Current Techniques of Analytical Chemistry was removed and a good grade was attained. How this occurred is beyond me at present.
Inasmuch as I was busy with course work and Galla was working part-time, we did not have much of a life socially. Of course we had neighbors that we knew and we had some contacts with some of the graduate chemistry students. We did play bridge at the Memorial Union some evenings with faculty and staff members. I still have stashed away some American Contract Bridge League Master Point Certificates stating how many fractional points we had won. However, we were and still not members of the bridge league.
To some extent I needed to find some form of distraction from school work, so I purchased some oil paints, brushes and boards. Although I did not accomplish much, it was relaxing to try prodcing some scenery on a board. We still had the Argus 35 mm film camera and we did take photographs around our living area.
By the end of this semester I was hard at work relearning French and learning scientific German so that I could get the language requirements out of the way. The modern language department gave the tests. One had to translate a scientific article in each of the languages selected to meet the requirement. I did not pass the tests the first time, but we were given a second chance and this time I did pass both language exams. I also was hard at work studying for the preliminary exams in the major and minors. During the summer of 1949 I took the following courses: Chem 293 Reaction Mechanisms and Research in Chem. Sometime between the end of the semester and the end of the summer session I took the preliminary written three-hour exams. I passed the analytical and organic chemistry exams with high grades and I barely made it with the physical chemistry exam. Now I needed to have a committee selected for my preliminary oral exam, and here there were some unexpected events. The events between the time I passed the preliminary written exams and the preliminary oral exam, that I eventually passed, were initiated because of my performance in the research area and my relationship with Dr. Elving.
NOTE SUN OCT 03 2010 THE FOLLOWING PARAGRAPH NEEDS TO BE REWRITTEN To write about my performance in the research requirement for the Ph.D. degree, it will be helpful for the reader to gain some understanding of the field of polarography. The following two sections of this chapter will attempt to provide the reader an elementary understanding of an electrochemical cell and then the dropping mercury electrode in an electrolysis cell. It will be understandable of the reader will skip the next two sections and continue reading the autobiographical narrative.
NOTE SUN OCT 03 2010 THE NEXT SECTION AS DELETED ON THIS DAY
NOTE SUN OCT 03 2010 The next section on polarography needs revising. Start with some description of the metal mercury.
Polarography is an electrochemical method of analyzing solutions of reducible or oxidizable substances. It was invented by a Czech chemist Jaroslav Heyrovsky in 1922 and then developed by the professor and a group of chemists. Professor Heyrovsky was awarded many honors and in 1959 won the Nobel Prize. Two books that I still have are Polarographie, by Professor Dr. J. Heyrovsky, published in 1941 and Polarography, by I.M. Kolthoff and J.J. Lingane, published in 1946 (Revised reprint from the book published in 1941). Dr. Heyrovsky’s book is written in German and I managed to translate parts of it when I had to do so.
During his thesis defense at Prague University (1918), Heyrovsky met Prof. Kucera, who invited Heyrovskýý to join his research group to study the dropping mercury electrode (DME) for electrocapillary measurements. From 1921, Heyrovsky applied himself to the intensive study and interpretation of electrocapillary curves. On 10th February 1922, he used a mercury dropping electrode for electrolysis in his researches, which had been inspired by Prof. B. Kucera back in 1918, and so laid the foundations for a new scientific discipline - polarography. Shortly thereafter, with his Japanese colleague, Masuzo Shikata, he constructed the first instrument for the automatic recording of polarographic curves, which became world famous later as the polarograph.
An electrochemical cell, or galvanic cell, is one in which an oxidation-reduction reaction produces an electric current. Electrolysis may be defined as the occurrence of chemical reactions, under the influence of an electromotive force (voltage), at electrodes immersed in solutions. In any electrolysis cell, the reaction at one electrode is an electroreduction (cathode), and exactly an equivalent amount of electrooxidation takes place at the other electrode (anode). in reverse, in an electrolysis cell is one in which electrical energy is used to bring about an oxidation-reduction reaction. Polarography, also called polarographic analysis, or voltammetry, is based on the measurement of the current that flows through a solution as an increasingly larger voltage (usually negative) is applied to an electrode in an electrolytic cell. The method is based on the interpretation of the current-voltage curves that are obtained when electroreducible or electrooxidizable substances are electrolyzed in a cell in which one electrode consists of mercury dropping dropwise from a very fine bore capillary glass tube. From the unique characteristics of such current-voltage curves both the species and concentration of the electroreducible or electrooxidizable substances present in the solution can be determined.
A typical arrangement for obtaining current-voltage curves with the dropping mercury electrode is shown schematically in Figure 1. In this diagram, A is the electrolysis cell containing the solution to be analyzed , B is the dropping mercury electrode, and C is a stationary pool of mercury on the bottom of the cell which serves as the second electrode. The dropping electrode consists of a drawn out capillary tube, whose internal diameter at the tip is about 0.03 mm, connected to a reservoir of mercury. Mercury drops issue from the capillary at the rate of about one drop every two to four seconds. The drops are very small, having a maximum diameter at the breaking point of about only 0.5 mm. The cell is connected in series with a calibrated galvanometer G ( measure current), to a battery (or other source of direct current) and a rheostat, by means of which a voltage can be applied to the cell. Current-voltage curves are obtained by gradually increasing the applied voltage and noting the current indicated by the galvanometer. The current is ordinarily quite small, seldom exceeding 50 microamperes.
Since oxygen is readily reduced at the dropping mercury electrode, and usually interferes with with the current-voltage curves of other substances, it is generally necessary to remove dissolved air from the solution to be elctrolyzed, by bubbling an inert gas (like nitrogen) through the cell before, but not during, the electrolysis.
A typical cathodic current-voltage curve shown in Fig. 2 was obtained by electrolyzing an air-free solution of 0.0013 M zinc sulfate in 0.1 N potassium chloride. In this figure the applied voltage is plotted on the x-axis, and the corresponding current on the y-axis of a sheet of graph paper. It should be noted that that only an exceedingly small current , the “residual current,”flowed through the cell until the decomposition potential was reached at an applied electromotive force of about 1.0 volts. When the decomposition voltage was exceeded continuous electrolysis began, consisting of the discharge of zinc ions at the dropping mercury cathode to form an extremely dilute zinc amalgam , and the anodic dissolution of mercury , with the subsequent formation of calomel, at the large quiet anode. It should be noted that the current did not increase indefinitely with the increasing applied voltage after the decompostion potential was exceeded, but gradually approached a limiting value and finally became constant and independent of further increase in the applied voltage. Under optimum conditions, and all other factors constant, the limiting current is directly proportional to the concentration of the electroreducible substance. This fact is the basis of quantitative polarographic analyses.
The limiting current is caused by a virtually complete state of concentration polarization at the dropping mercury electrode. As a result of the discharge process, the concentration of the reducible material is depleted close to the surface of the dropping mercury electrode, and this loss is compensated by diffusion of a fresh supply of reducible material from the body of the solution. The rate of diffusion depends directly on the difference in concentration between the depleted surface layer and the body of the solution. As the voltage is increased above the decomposition potential and the current increases, the average concentration of the reducible substance at the surface of the mercury drops decreases, and the rate of diffusion is correspondingly increased. As the applied voltage is further increased, the concentration at the surface of the mercury drops becomes so small compared to the concentration in the bulk of the solution that the difference in concentration approaches a constant average value, equal simply to the concentration in the solution, and hence the rate of diffusion also becomes constant and practically independent of further increase in the applied voltage. With an excess of some indifferent salt present in the solution, the limiting current is determined practically entirely by the rate of diffusion and hence is called a diffusion current. Since the rate of diffusion attains a constant value, which is directly proportional to the concentration in the bulk of the solution, it is readily understandable why the diffusion current is directly proportional to the concentration in the body of the solution.
It should be mentioned that the necessary conditions that must be fulfilled to obtain a limiting current are that at least one electrode of the cell be very small, and the concentration of the reducible substance be not too large. That is, conditions much be such as to favor the attainment of an extreme state of concentration polarization
The (average) current observed with the dropping mercury electrode becomes steady immediately at each new setting of the applied voltage and is independent of the time of electrolysis This favorable behavior of the dropping mercury electrode is due to the fact that a fresh mercury surface is continuously being exposed by the rowing drops; the phenomena at a given drop are exactly duplicated at its successor. Hence the current at any point on the current-voltage curve is solely a function of the potential of the dropping mercury electrode, and is independent of the previously course of the electrolysis, or the length of time that the current has passed. A current-voltage curve obtained by increasing the voltage in the usual way will generally be retraced exactly if the applied voltage is gradually decreased to zero.
The dropping mercury electrode is generally as a cathode (electroreduction). The reason for using a relatively large, quiet pool of mercury as the second electrode of the cell (usually as anode) is that such an electrode remains practically depolarized when the solution contains halides (sodium chloride, potassium chloride, etc.) Or other ions which form insoluble salts with mercury. It thus retains a practically constant potential independent of the applied voltage, and only the dropping mercury electrode becomes polarized. For example, in solutions of chlorides the quiet electrode acquires a potential practically equal to the potential of a calomel electrode.
The decomposition potential of a given solution is characteristic of the particular electroreducible substance present. Even more characteristic is the so-called half-wave potential, which , as its name implies, is the value of the applied voltage, or better the potential of the dropping mercury electrode against an external reference electrode, at that point on a current-voltage curve where the current is equal to one-half of its limiting value. In the contradistinction to the decomposition potential, which depends on the concentration of the reducible substance, the half-wave potential is in general independent of the concentration of the reducible substance, provided that the composition of the solution with respect to foreign salts is kept constant. The half-wave potention of a given substance is also independent of the particular capillary used, and the drop time.
My first assignment was to produce current-voltage curves for a number of nitro-alkane compounds in aqueous buffer solutions at various pH levels (degrees of acidity. The goal was to determine if these industrially important compound could be analyzed by polarographic techniques.
. I was assigned a Heyrovsky–Shikata polarograph which was manufactured in the United States by E.H. Sargent and Co., Chicago. This polarograph was invented in 1925. It automatically obtains and photographically records current voltage curves. Without going into detail, it is sufficient to state that this instrument automatically increases the voltage across the polarographic cell and records the corresponding currents on photographic paper, which is mounted on a revolving drum. Once a curent-voltage curve is recorded it was necessary to take the revolving drum into a dark room where the sheet of photographic paper is removed and developed. Of course, another sheet of photographic paper s mounted on the drum while in the dark room. After recording many current-voltage curves, it became apparent that on development the photographic paper shrank. This is one reason that we began to perceive inconsistent results.
One day, Dr. Elving came into the laboratory and introduced me to a visitor. The visitor was Dr. Grant Wernimont, who was a statistician employed by Kodak, in Rochester, New York. Dr. Wernimont was the first graduate student to receive his Ph.D. degree under the direction of Dr. DeVries. I told Dr. Wernimont about our photographic paper problem and he promised to send us paper that would have minimal shrinkage on development. Many years later, I was to meet Dr. Wernimont again and we worked together on a project of mutual interest.
Dr. Elving was a hard-driving individual, however, he was an excellent teacher. I had to write monthly reports of my research progress. Invariably, a report was criticized for its clarityy. I must say that when I wrote reports later in life, I felt that Dr. Elving was looking over my shoulder. There is one incident that is memorable. After having many reports essentially torn apart and rewritten, I took the last report, that had been corrected and rewritten, and just inserted new date numbers. Dr. Elving started to tear this report apart, so I said that that this was the corrected format from our last meeting. Dr. Elving then looked at me and said, I not always right.
It turned out that another glaring error that had been overlooked was also responsible for inconsistent results. This error had to do with the revolving drum. When the recording was stopped, it was assumed that the drum did stop revolving. This turned out not to be so; the drum revolved after the recording phase was stopped and this made the voltage measurements incorrect. Of course, I learned a lot, but my research effort did not please Dr. Elving, particularly, as grant money was involved.
Sometime after I had passed the written preliminary exams, Dr. Elving announced that he was leaving Purdue university for a position at Pennsylvania State University. Dr. Elving asked a number of his graduate students to join him, but I was not one that was invited. I suspect that had I been invited to go with Dr. Elving, I might have oped out as II do not think we wanted to resettle again before earing the degree. I want to add here that in one conversation with Dr. Elving, I was told that I did not have the temperament for research and that having a M.A. degree, I should look into the developing field of hospital laboratory chemistry. Dr. Elving was prophetic for I did end up in the hospital chemistry field (clinical chemistry or overseas, clinical biochemistry).
I had to decide upon another mentor for my research. I decided to ask Dr. Nathan Kornblum, Ph.D., Associate Professor of Organic Chemistry, to take me on as I was an organic chemistry major. Rachel Britton who left Columbia University to become a graduate student at Purdue University and Dr. Kornblum were married. When we first came t Purdue University, I renewed my acquaintanceship with Rachel. We were invited to spend an evening with Rachel and Dr. Kornblum. Rachel received her Ph.D. degree while working for Dr. Kornblum and she later made a name for herself in the field of chemical education. Unfortunately, Rachel died at an early age.
I was accepted as a graduate student by Dr. Kornblum. A committee for my preliminary oral exam was selected. Dr. Kornblum was the chairman as he would be my major professor; the other members of the committee were M.G. Mellon, Ph.D., Professor of Analytical Chemistry, Albert Rockin, Ph.D., Assistand Professor of General and Physical Chemistry, and the third member is completely forgotten. The oral exam was conducted in a large auditorium where the rows of seats were placed on an upward sloping floor. The faculty members were seated in front of me and I was at the blackboard in front of the room. Dr. Elving at one time said that oral exams were like indoor sports for the faculty members. He also said that one should try to get the faculty members into arguments with one another. However, alas, I did not know how to do this. The questioning by Dr. Mellon and the unknown member of the committee is not memorable. I had no problem with the abswers. It was Dr. Kornblum that was severe and by the time he got done with me, I felt like a wet rag. Then questions came from Dr. Rockin. Dr. Rockin had the 1320 page textbook of physical Chemistry by Samuel Glasstone on his lap and he seemed to flip pages here and there before asking a question. Then he asked me to draw a vapor pressure-composition diagram for a chloroform-water mixture. I got very little information and I struggled to come up with an answer. It turns out that he was looking at page 731 of the textbook; the chloroform-water mixture partially filled a donut shaped container so there were two surfaces of this mixture. I really was sweating as I just could not come up with the required diagram. Of course, had I realized the shape of the container i would have been able to answer the questions with more authority. I was sked to wait outside in the hall while thecommittee came to a conclusion. It was Dr. Mellon that gave me the news, not Dr. Kornblum. The committee was undecided and the recommendation was that I would have to take the oral exam over again.
On consultation with Dr. Kornblum after the oral exam, he told me that he would not give me any credit for the time I spent in research with Dr. Elving. This would mean that I would have to spend at least three or four more years at Purdue university. We did begin to like it living in West Lafayette, however, the G.I. Bill money was about to end and we might not be able to survive financially in a long haul.
Now that I think back about the last encounter, I realize that my next move was not very diplomatic. I am not sure that I actually told Dr. Kornblum about my next move. I decided that I would not work with Dr. Kornblum. I went to see Dr. DeVries and he was quite receptive in accepting me to continue my research under his direction. I was going to continue research in the field of polarography and Dr. DeVries stated that I would get credit for the time I spent with Dr. Elving. My research problem would entail polarography with nonaqueous solvents. I would now declare that my major subject was analytical chemistry and my minor subjects were organic and physical chemistry.
Anew committee was selected for my oral reexam. Dr. DeVries was the chairman of the committee, and the other members were Dr. M.G. Mellon, Dr. William Truce, Ph.D., Associate Professor of Organic Chemistry, and Dr. Walter Edgell, Ph.D., Professor of Physical Chemistry. The oral exam took place during the fall season. It was held in Dr. Elvings old office. A fewquestions are memorable. Dr. Edgell noted that I had a Crosley, so he began questioning me about the heat developed when the rngine was running. Then Dr. Edgell wanted me to develope the equation describing the refrigerator. I knew the equations for the heat engine, so the refrigerator had me hemming and hawing. I was given a break midway and while I was standing out in the hall, Dr. DeVries came over to me and said I was doing well. This was gratifying. I did pass this oral exam.
After leaving the oral exam area, I was elated but very tired. To recuperate from the stress of the recent events, Galla and I decided to get away for several days. We drove to the Mammoth Caves in Kentucky. We stayed in a lodge near the caves. We did take a tour of the caves before driving north again. We thought that we would like to make a stop in Brown County which is in the southern part of Indiana. The colors of the leaves were supposed to be spectacular in Brown County in the fall. According to a road map, there was a car ferry to cross the Ohio River on a direct route to Brown County. Both Galla and I were used to the Staten Island Ferry terminals in New York City, so we expected to see some sort of similar structures at the Ohio River. When we arrived at the Ohio River, we were on top of a bluff, and there was a sign stating that to get the ferry, blow the car horn and drive down the road to the beach. After sounding the horn we saw a small flat boat coming across the river. I was dubious aboutdriving down the rough road to the shore, but I did. We drove onto this boat that took us tothe shore in Indiana. We drove off the boat onto a country road surrounded by flat fields. I believe itwas raining when we arrived at a parl lodge. After a walk and an overnight stay we drove back to West Lafayette.
The Light at the End of the Tunnel
I was now an official candidate for the Ph.D. degree. The last requirements were to emerge with a thesis showing the results of some original research and a defense of the thesis. The courses I took during the fall of 1949 was Chem 299 Research in Chem. It was during the winter of 1950 that I took the courses Chem 274 Absorption Spectroscopy, Chem 252 Emission Spectrometry, and Chem 299 Research in Chem.
Dr. Mellon taught the absorption spectroscopy course. It was a lecture course and there were no exams as I recall. Dr. Mellon’s book Analytical Absorption Spectroscopy was published in time for this course. It was an excellent textbook and it served as a reference book for many years to come. An updated edition never came about. Dr. DeVries taught the emission spectroscopy course. The optical part of the emission spectroscope was a very large oblong box on its side. We actually performed experiments and we had unknowns to identify. This course was very interesting and it was appreciated when later on I had to send samples out for emission spectral analysis. During the summer of 1950 I took the courses Chem 278 Electrochemistry Chem 299 Research in Chem. I was taking this course again and Dr. DeVries was the instructor again. By this time the material had finally penetrated my mind and I understood the material fairly well.
I was assigned bench space in a large laboratory on the street floor. My lab companions whose research was being mentored by Dr. DeVries were Don Cohen, Jacob (Jake) Sedlet, and Jonathan Amy. Don was in the last stages of earning the Ph.D. degree, Jake had some time to go as I did, and Jonathan had just joined the group. Jonathan had been a radio man in the Merchant Marine during World War II. He started his research with Dr. DeVries, but he ended up getting the Ph.D. by working with Dr. Edgell. Jonathan and his wife purchased land close to the Wabash River and we visited back and forth with them this year. We also had social relations with jake and his wife.
There was music hall on campus and it was claimed that this theater had six mire seats than the Radio City Music Hall in New York City. I believe that we went to several shows. One show that stands out is when Danny Kaye performed in the Music Hall. There were many encores and finally Danny Kaye came to the side of the stage and sat down on a stairway into the theater from the stage. He finallt said he was tired and the show finally ended with lots of loud applause.
However, most of the year was devoted to my research project. There were time-consuming procedures which made it necessary for me to be in the lab late at night many times. There were other graduate students around working in the labs during the night and while waiting for some process to end there were penny ante poker games. Of course this was against the rules of the university.. But most of thegraduate students were veterans, so they thought they had privileges. No one ever bothered us while the gaes went on.
As Dr. DeVries did not have a grant for my research project, I had to scrounge around for lab equipment and chemicals. I was able to locate and appropriate a large metal tray; this item was needed as large quantities of mercury could possibly be spilled from the reservoir above the capillary of the dropping mercury electrode set-up. To complete my need for equipment I need an H-electrochemical cell and a glass component of a thermostat for maintaining a constant water bath temperature. I drew up specifications for the H-cell and the thermostat for the department glass worker. I was told by Don and Jake that Dr. DeVries would not O.K. a request for glass working. I would have to make my own glass equipment. This I did; they may not have looked as they were made by a professional glass worker, but they were adequate for my research project. The illustrations below are representative of my H-cell set-up and the polarograph, the Electdrpode. .
The Electropode was an instrument operated manually. I had to set the voltage and record each corresponding current reading in my laboratory notebook. Then I had to plot the data foreach polarogram on graph paper. This was a tedious and time-consuming procedure.
We decided to do polarographic studies of nitroethane, 1- and 2-nitropropane, 1- and 2-nitrobutane, 1,3-dinitropropane, 1,5-dinitropentane, 2,2-dimethyl-1,3-dinitropropane, 2,2-dinitropropane, and n-butylnitrate. The solvents used in this study were methanol, 1 to 1 methanol-benzene mixtures, methanol-glycerol mixtures of varying concentrations, isobutyl alcohol, ethylene glycol, , and glycerol. Lithium chloride was used as the supporting electrolyte in concentrations varying from 0.2 to 0.5M.
Needless to say, much time was spent in obtaining and purifying the chemicals. Many a day and night were spent in the laboratory waiting for equilibrium to occur in distillation columns and then taking off small fractions of purified distillate. Because much time has passed since I engaged in this research, I have a smattering of visions of using sodium metal in some purification process. Sodium will have a violent reacion when exposed to water so bars of this element are kept in kerosene. And then in the polarographic process itself, oxygen had to be removed by passing nitrogen through an acetic acid solution of chromous chloride to ensure oxygen-free nitrogen, and then through the solution in the H-cell. Used mercury, and there was lots of mercury used in this study, had to be purified by bubbling nitric acid through a large batch, in a large flask, for about 24 hours.
There is one incident that cannot be forgotten. The tray holding the cell set-up was near a sink. One morning while washing some glassware my hand brushed against the tray and I felt some sort of tingle. Without thinking, I put the palm on my hand on the tray and I was hit with quite an electric shock. Jake came in the lab at the time I did this and he remarked that my face was green. The electric motor I had been able to get for stirring the water in the constant-temperature bath had a exposed wire. With use the wire became exposed enough to electrify the ring stand it was mounted on and the metal tray. This was a shocking way to enhance a learning
I got a nice break when Dr. DeVries let me know that he was able to get the automatic recording Leeds & Northrup Type E Electrochemograph
This instrument certainly made life easier as the I did not have to plot current-voltage curves anymore. The time-limiting factor was making up the proper solutions to be analyzed. The use of this instrument enabled me to generate much data in a relatively short time period.
By the summer of 1950 I had generated data that indicated that nonaqueous solvents could be used for the polarographic analysis of organic compounds that were insoluble in aqueous solutions. Dr. DeVries decided that I should write my thesis. This I did during the beginning of the summer. There were many figures to be drawn for the thesis and there were no such things around as the personal computer I am now using to write this autobiography. I had to learn drafting techniques and I spent many hours over a drawing board getting figures ready for publication.
I submitted my thesis and I was told by Dr. DeVries that as far as he was concerned I would be awarded the Ph.D. degree by the end of the summer session. Then came a shock.
Dr. DeVries told me that a new committee had been appointed over his objections. Then new committee was made up of more than the usual four members and it included Herbert Brown, the future Nobel Prize winner. This committee decided that I should stay and continue working toward the degree. There were internal faculty politics involved as some Professors kept graduate students for many years before deciding that they had earned their degree. After all, this was cheap labor. Also, there were overtones that Dr. Kornblum had a hand in this decision.
At Last, the Quest is Rewarded: September 1950 through January 1951
When I submitted my thesis, I had no job in sight, but we decided that I would start looking for work at the Chicago fall national meeting of the American Chemical Society. We started to pack personal belongings in boxes. We also sold our furniture to new residents in our area. We moved our bed into the living room and moved the packed boxes into the bedroom. I believe all we had left were the kitchen table and two chairs beside the bed and refrigerator. So for this time interval our home was rather bare. We did appropriate red bricks and made some bookcases with some unpainted boards. I put the drawing board on the top of some of our packed boxes and this served as a desk.
Our financial situation was not very good at this time. The G.I. Bill monthly stipend had come to an end. I did have the monthly compensation check from the Veterans Administration, however, it had been reduced because my disability percentage had been reduced from 40% to 20%. I was able to get a teaching assistantship for the fall semester of 1950. Sometime at the beginning of the semester, Galla quit working part-time in the statistics departmet/ I suspect that we were drawing some capital from our bank account.
On the lighter side, it was on a Saturday in September that we drove to Indianapolis for a buffet lunch at one of the hotels and then we wandered around in a department store. We came upon an area with television sets. Television was in its infancy and not a common household item. Seeing that the Purdue University-Notre Dame football game was in progress, we stopped to watch it. We ended up sitting on the floor with many other onlookers to watch this game. The Purdue-Notre Dame and Purdue-Indiana football games are examples of intrastate rivalries. During the week before we drove to Indianapolis, students were all excited about the game because Notre Dame’s team had won about 38 or 39 straight games and even though Notre Dame was expected to beat Purdue’s young team easly. Needless to say, Purdue won the game. Students paraded up and down through Monday. The University President said that Monday was not a university holiday, but the students could keep celebrating. The coach got up at a rally and said, “If we don’t win another game this year, the hell with it.” Purdue lost every game until the end of the season when the team beat the Indiana university team.
I believe that during my last semester at Purdue University, I took a seminar course and of course, chem research. It seems to me that I prepared an hour lecture on neutron activation analysis. I gave the lecture one evening and I believe Galla came to hear what I had to say.
As for my research project, I continued my work in the laboratory. After a lengthy discussion with Dr. DeVries we decided to measure the viscosities of the solvents I used Thus we would be able to study the effect on the diffusion current by the viscosity of the solvents.
I used a Hoeppler viscometer for measuring viscosities. The Haake Falling Ball Viscometer is illustrated in the figure and it is essentially an updated version of the Hoeppler viscometer. The
inner glass tube of the device is filled with the solvent to be measured (orange area in the figure). There is an outer chamber through which water at a particular temperature is circulated. There are two marks on the inner tube; one mark is close to the top and the second mark is close to the bottom of the tube. A glass ball is dropped into the inner tube and using a stop watch the time interval between the two marks is noted. The viscosity is calculated by comparing the time interval to one in a n established standard. Imagine my surprise when I dropped the glass ball through one of my solvent mixtures and the ball was not to be seen. I know that I found a way to visualize the falling ball through this solvent mixture, but as I write this more than 54 years later, I have no idea how I accomplished this task. For calculation purposes, I had to measure the densities of each of the solvent mixtures and that was with a Westphal balance. With this type of balance we can measure the density of a liquid. With riders, placed opportunely on the rider scale, we compensate the decrease of the weight of the plummet when it is completely immersed in the liquid. A comparison is then made with a liquid of known density.
It was toward the end of the semester when Dr. DeVries told me to add my newly generated data to the thesis and he would resubmit a rough draft to the committee again. It was probably on a Saturday when Galla and I went over to the statistics department where we were able to use two motor driven mechanical calculators. At this time there were three prominent mechanical calculators and they were the Monroe, Friden and SCM Marchant. I had many, many calculations to perform and it certainly was wonderful to have the use of a meachanical calculator. I am not sure if I used a Friden or a Marchant for my calculations, but it sure beat the use of a slide rule or paper and pencil. Galla used a like calculator and repeated my calculations to ensure that the results would be correct. Then there was the task of more figures and text, all of which were done on my makeshift drawing board desk in our fairly empty apartment. It was before the end-of-year holidays that I was informed that my thesis was accepted. Now I had to have multiple copies typed and that was done with a top copy of a good grade of paper and copies were made by inserting carbon paper between onion skin paper. Not being adept as a typist we had to have a professional typist do the typing and it might have cost ten cents a page. Then the original copy and the onion skin paper copies had to be bound. I do not remember the total cost, but I suspect that it was considerable in relation to our total monetary assets.
My final oral exam where I would defend my thesis was scheduled for Saturday morning, January 20, 1951. My committee now consisted of Dr. DeVries, Dr. Herbert Brown, Dr. William Truce and Dr. Walter Edgell. When I arrived at the chemistry building, only Dr. DeVries was waiting for me. Dr. DeVries had to make telephone calls to remind the committee members that they were scheduled for my final oral exam. Both Dr. Brown and Dr. Truce said that they would sign-off on the thesis and would not attend the oral defense. Dr. Edgell said he would come for the exam and we had to wait a while for his presence. Finally, we ended up in an empty classroom and I presented an abstract of my thesis. Very few questions were asked. I brought up something about the modern theory of the rates of reactions and Dr. Edgell asked me to amplify my remarks. Anyway, what seemed like an eternity to and in reality it was a very short time interval, I was asked to wait outside of the classroom. In a few minutes Dr. Edgell walked out and put his arm around my shoulder and said something to the effect that I was now a Ph.D. and I will all the benefits of that degree even though he wasn’t sure what the benefits were. Actually, the benefits are the prestige of having earned the Ph.D. degree and it would also have monetary rewards.
It might be of interest at this time to write about any impact my research may have had. First, It was in September or October of 1950 that Galla and I attended the annual fall national meeting, in Chicago, of the American Chemical Society At this meeting, Dr. DeVries presented a paper based on my research work up to that time. Dr. DeVries also presented an abstract from my thesis at the Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, March 5, 1951. An abstract of my thesis was published in the American Chemical Society Journal in 1952 (Radin N, DeVries T. Some aliphatic nitro compounds and n-butyl nitrate in nonaqueous solvents. Polarographic study. Anal Chem 1952;24:971-3). Dr. DeVries sent me a batch of reprints ;I never received a request from anyone for me to send them a reprint of the paper. The reprints have turned yellow from the aging process. Sometime in the decade of the ‘80s, I found a paper in which a research in Canada had repeated my work. Also, I read the text of an award lecture with an autobiographical preface. This lecture had been given by Professor John Stock, Professor of Analytical Chemistry Emeritus at the University of Connecticut. John Stock was originally from England and in his autobiography he stated tha he had used the polarograph while working as an industrial chemist. Inasmuch as I had been communicating with John Stock during the decade of the ‘90s, I sent him a reprint of my paper. In a letter from John Stock, he stated that he knew about my work back in England as my paper helped him solve a problem. In a way this was gratifying as my work had not been a wasted effort.
Kolthoff IM, Lingane JJ. PolarogrphyNew York, Unterscience Publishers, Inc.,
With the hope that I would finish my graduate studies by the end of the semester in January, I began to look around for possible employment. I needed to get job as soon as possible our assets were quickly heading toward zero. As far as I understood it, jobs were not easy to get and a job that would pay about $5,000 annually would be a good find. I was interested in teaching at a college or university or a Federal Civil Service job as it offered much security for the future. The way to end up as a university faculty member was to try to det a post-doctoral position with a faculty member of a university. Then when I thought about this way to go, I did know that the adage publish or perish meant that as a faculty member one had to bring in grant money to support research programs. Personnel staff members from various organizations did visit Purdue university to recruit for jobs. I had one interview for a position as a faculty member at Colby College in maine, but I did not follow-up on that one is it paid a bit more than $3,000 annually. The one interview of interest was with a Dr. S from the National bureau of Standards. This was a civil service type of job and at that time expenses were paid for an interview of a candidate at the job site. Dr. S suggested that I should come to Washington, DC at the time of the end-of-year holiday and he would arrange for me to be interviewed in several departments. This I eventually accepted and I also submitted an employment application to the Federal Civil Service Commission offices. This way I would get a grade and to this grade points would be added as I was a veteran.
So, sometime in December we drove east to Washington, DC. I stopped at the National Institutes of Health, in Bethesda, Maryland, and left an application for employment at the personnel office. I was not encouraged by the the response that if there is an opening sometime we will look at your application. The I spent some time at the National Bureau of Standards. Dr. S had arranged for me to have interviews with a number of staff members. I met John Taylor, who was heading a polarography group. I was told it would be nice having you, but there are no openings. I had somewhat the same response in a spectroscopy laboratory. Then I had a conversation with D. B,, who headed a silica chemistry study group. Yes, there was an opening, but it may take months to process my application for employment. I was told promotions to higher grade levels was slow as one had to wait for someone in the group to retire before there was any movement. I could not get excited about silica chemistry, so I did no follow-up of any employment at the National bureau of Standards.
We headed for New York City and stayed with Galla’s parents in their house in Fort Wadsworth, Staten Island. Galla and I had applied and received tickets to attend the $64 Question radio quiz show. Before the show started, categories of questions to be asked were announced and for each category a member of the audience was selected to vie for a cash prize. As far as I could ascertain at present, If a contestant answered the first question of a particular category correctly it would be worth $1.00. The cash prize doubled each time a question was answered correctly and the maximum a contestant could earn was $64. A category of famous fathers was announced and the host of the show announced that the father of the youngest child in the audience would be selected for tha famous father category. Some raised their hands and announced the age of their child. Galla poked me and got me to raise my hand. Galla was pregnant and I told the show host that she was expecting. I was asked when. I said May of next year. The host announced minus five, come on up. We both went up on the stage and before we were quizzed, we were told what the first three or four questions were and we were given the answers. Well, these were the questions we answered correctly while on the air, however, we could not answer the next question correctly. Now comes a mystery. We were given $100.00 Either we were on another radio quiz show or there was some kind of bonus or just appearing as a contestants. Both Galla and I agree that we did get the $100. The money we won was a bonanza for it paid for our trip and then some.
Before returning to Indiana, Marty was brave enough to ride in the back seat of our Crosley as we drove to the Norwalk area, Connecticut, for us to have dinner with Abe and Lynn Savitzky. Abe had earned his Ph.D. at Columbia University with his major in physical chemistry. Abe’s research had something to do with developments in the field of infrared instrumentation and he was now employed by the Perkin-Elmer Corporation, a laboratory instrument manufacturer. It was a cold winter night. The moment we stepped into their house, Lynn greeted Galla with, “When are you expecting.” We did have a very nice evening together before driving back to New York City. Galla has not seen Lynn since that evening. Man, many years later, when I was an instructor at a workshop at the Department of Health in Hartford, Connecticut, I was able to visit Abe and Lynn as I made a stop at their home on my way to New York City. Then sometime in the decade of the’90s, while Abe was in Atlanta, Georgia for a technical meeting we had dinner with him and then spent some time with him and several of our friends at our home. .
Our trip back to West Lafayette is memorable. After the beginning of the new year (January, 1961), on leaving Staten Island, we drove to Lakewood, New Jersey and we stayed overnight at my father’s farm. It was before dawn that we began to drive back to West Lafayette. The New Jersey state highway to Philadelphia was icy due to the freezing rain which had started to fall during the night. It was still dark when I thought the highway had veered to the right and as I steered right, I realized that this was just an intersecting road, not the highway route I should have continued to drive on. I hit the brake, and that was a mistake as we spun around, and fortunately we ended up off the road at this intersection. We continued to drive on and finally we were able to navigate through Philadelphia. Then we headed for the start of the Pennsylvania Turnpike, which at that time was at King of Prussia (northwest of Philadelphia0. When I started to drive down a steep two-lane suburban road the Crosley spun around and we ended up in the right lane, only we were pointed toward the top of the hill. I decided to try and go downhill cautiously by driving in reverse, when a man came out from between some tall bushes and motioned for us to stop. This I did. We were told that because of the icy conditions, it would be impossible to drive uphill. I told the man we were trying to drive downhill. We got a queer look and it was suggested that we should pull over and wait for the ice to thaw. We did pull over for a while and I decided to try going down hill again only this time driving forward. We did make it this time and while driving on the Pennsylvania Turnpike, I kept feeling that we were going to slide or spin around. We made it to the Pittsburgh area where we stopped for the night. The rest of the trip was uneventful.
When we returned to West Lafayette, it was time to get ready to leave the area permnently. I had no idea of where we were going to go. At his time, I suspect that we were planning to stay with Galla’s parents until I found employment. All I had to do now is wait for my thesis to be readied and I probably cleared out my laboratory bench area.
Sometime early in January, I was summoned to answer a telephone call. The call was being made by a Mr. B., who was on the staff of the Engineering Research &Development Laboratories, Fort Belvoir, Virginia. I was stunned by the caller. He asked when I could come to work at the labs. My application for employment at the Federal Civil Service Commission offices had been looked at and it seemed that I would fit the needs of the labs. I really did not relish working for the Department of the Army. But I needed a job. So, I put off accepting the position by suggesting that I visit the labs before accepting the job. We made a tentative date. So, now, we would head for the Washington, DC area after leaving Purdue University. I had also written a letter in response to an employment wanted ad in the American Chemical Society Chemical & Engineering News; the offer was by the Federal Sanitary Center, in Cincinnati, Ohio, for a chemist to test the radioactivity at the headwaters of the Columbia River, in the state of Washington. I made an appointment to stop at the center for an interview when we driving to see about the position at Fort Belvoir.
We had decided not to attend the graduation ceremonies at the end of January. Today, I still regret this decision for that might have been the only time I would have gotten to wear the hood for a Ph.D. at graduation rites. Neither Galla and I can recall how we handled the last of our personal possessions since we really had no address where to send them. I suspect that boxes of books and other items plus our bed was picked up for storage by a local moving company until we could provide an address. We are not sure as to what we did with our refrigerator; I suspect that we sold it.
After I passed my final oral exam on Saturday, we left our barracks apartment on my birthday, Monday, January 22, 1951. We packed as many boxes of personal items into the Crosley sedan as we could. We drove to Cincinnati, I was so proud of the Ph.D. degree I earned, that when we stopped in front of a hotel where Galla would go to inquire about getting a room for the night, I suggested that she should register as Mrs. Dr. Radin.
The next morning I went to the U.S. Public Health Environmental Health Center. During the discussion of the position that was advertised, I remarked that it might be difficult for us to settle down in Washington as our families were living in the eastern part of the country. I was told that there were other positions open at the center itself. One obstacle remained. It would two to three months to process m civil service application before a concrete offer could be made. I left the center without a definite commitment to wait for an offer. We left for Virginia.