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 II 
 
 
URBANA 
 
STATE OF ILLINOIS 
 
 DWIGHT H. GREEN, Governor 
 
 DEPARTMENT OF REGISTRATION AND EDUCATION 
 
 FRANK G. THOMPSON, Director 
 
 STATE 
 
 DIVISION OF THE 
 
 GEOLOGICAL 
 
 M. M. LEIGHTON, Chief 
 URBANA 
 
 SURVEY 
 
 CIRCULAR NO. 68 
 
 SOME STUDIES PRESENTED AT THE STATE 
 ACADEMY OF SCIENCE IN 1940 
 
 Reprinted From the Transactions, 
 illinois state academy of science, 
 vol. 33, no. 2, December 1940 (1941) 
 
 PRINTED BY AUTHORITY OF THE STATE OF ILLINOIS 
 
 URBANA, ILLINOIS 
 1941 
 
>7 
 (A-42809) 
 
CONTENTS 
 
 PAGE 
 
 FUSAIN CONTENT OF FINE SIZES OF ILLINOIS COAL, Bryan C. Parks and 
 L. C. McCabe 5 
 
 PRE-GLACIAL RIVER TICONA, H. B. Willman 9 
 
 AERIAL PHOTOGRAPHY, Harry McDermith 13 
 
 THE USE OF PIPETTE ANALYSIS IN CLAY RESEARCH, Richards A. Row- 
 land 15 
 
 THE INTRODUCTION OF FLUORINE INTO AROMATIC NUCLEI BY MEANS 
 OF AMMONIUM FLUOBORATE, G. C. Finger and F. H. Reed 17 
 
 2-CHLORO-3, 5-BIS (ACETYLAMINO) TOLUENE, G. R. Yohe 18 
 
Digitized by the Internet Archive 
 
 in 2012 with funding from 
 
 University of Illinois Urbana-Champaign 
 
 http://archive.org/details/somestudiesprese68illi 
 
Geology — 19J/.0 Meeting 
 
 FUSAIN CONTENT OF FINE SIZES OF ILLINOIS COAL 
 
 Bryan C. Parks and L. C. McCabe 
 
 State Geological Survey, Urbana, Illinois 
 
 During the past ten years some notable 
 changes in coal preparation have taken 
 place, particularly in the smaller sizes. 
 The wide spread use of the domestic 
 stoker and the demand for better fuel for 
 it are largely responsible for these 
 changes. It is now common practice to 
 dedust, wash, dry, and dust-proof the 
 stoker sizes. The consumer receives a 
 cleaner, more uniform fuel as a result 
 but its preparation leaves the producer 
 with a serious waste problem as yet un- 
 solved. 
 
 In the most common process of de- 
 dusting, the coal is carried through an air 
 column in which the dust smaller than 
 10 mesh (1.65 mm) or 48 mesh (.3 mm) 
 is removed. Where the coal is wet 
 washed without dedusting, the coal finer 
 than 48 mesh is carried into the settling 
 pond and is lost. 
 
 There is only a limited market for de- 
 duster dust in cement and powdered fuel 
 plants, and the market value is below the 
 average cost of producing coal. Other 
 serious difficulties are encountered in the 
 transportation and handling of deduster 
 
 dust. At one mine 200,000 tons are 
 stacked on the ground (fig. 1), but at 
 mines where storage facilities are lacking 
 the dust must be hauled away, in one in- 
 stance, at a cost of thirty-five cents per 
 ton. 
 
 The authors estimate that 1,000,000 
 tons of dust are produced each year at 
 Illinois preparation plants at the present 
 time. Assuming the production cost to 
 be $1.76 per ton (the Bituminous Coal 
 Commission's average cost of production 
 for Illinois) the mining cost is over 
 $1,750,000. Storing or hauling on the 
 surface adds to the total cost. At many 
 mines the carbon sizes (minus % in.), 
 made in normal screening procedure, sell 
 in the market below the cost of produc- 
 tion. Between seven and ten million tons 
 of these sizes are produced. 
 
 By coking or briquetting, it may be pos- 
 sible to convert this waste or low-priced 
 coal into satisfactory smokeless fuel 
 which will bear a proportionate share in 
 the price structure. As the composition 
 of the raw coal determines the charac- 
 teristics of the coke or briquettes, a pet- 
 
 Fig. 1. — Coal dust storage at an Illinois Mine. 
 
Illinois State Academy of Science Transactions 
 
 CHEMICAL COMPOSITION OF BANDED INGREDIENTS 
 (DRY BASIS) 
 
 VITRAIN CLARAIN FUSAIN 
 
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 COAL MEASURES NV 1 ' """ | * J 
 MINES SAMPLED V^ 3 *? ■■■' vfcS 
 
 
 
 
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 MINES SAMPLED IN FUSAIN INVESTIGATION 
 
 Fig. 4. 
 
 rographic study of the dust and the car- 
 bon sizes was undertaken during the past 
 year. 
 
 Fig. 2 illustrates the chemical compo- 
 sition of the three most important con- 
 stituents of Illinois coal. Fusain differs 
 greatly from the other two ingredients 
 in that it has a very high per cent of 
 fixed carbon. While vitrain and clarain 
 readily agglutinate or coke, fusain exhibits 
 no such tendency. Fusain is character- 
 istically acicular or needle like in shape 
 while clarain and vitrain are granular. 
 (Fig. 3.) 
 
 In coking or briquetting the presence 
 of some fusain has been found experi- 
 mentally to be beneficial. The addition 
 of small amounts of fusain 1 tends to give 
 more blocky and less fractured coke. 
 According to Piersol 2 the addition of up 
 to 5 per cent of fusain increases the 
 strength of briquettes made from high vi- 
 train coal, and high fusain (up to 20 per 
 cent) coals produce briquettes having re- 
 duced smokiness. It is therefore desir- 
 able to maintain control of the amount 
 of fusain in the charge to the coke oven 
 or briquetting machine. 
 
 It was the purpose of this study to de- 
 
 termine the fusain content of the waste 
 or low-priced fine sizes of coal described 
 above, thereby to establish a basis for 
 determining the effect of definite quanti- 
 ties of fusain, first upon the effectiveness 
 of the briquetting process, and second 
 upon the combustion properties of the 
 briquette. Such information would per- 
 mit the selection of sizes of coal most 
 suitable for briquette production. The 
 present paper describes the methods of 
 study and certain incidental results. 
 
 During this investigation samples were 
 secured at 42 mines. A county outline 
 map of Illinois (fig. 4) shows the 
 boundary of the "Coal Measures" and the 
 location of 19 mines at which the 27 
 samples studied to date were obtained. 
 The two mines shown in Saline County 
 are operating in No. 5 coal. All other 
 mines shown on this map are operating 
 in No. 6 coal with the exception of the 
 Vermilion County mine which is in the 
 Grape Creek bed. 
 
 The following types of waste and low- 
 priced fine coals were secured at the 
 mines in sample containers holding from 
 10 to 50 pounds of material: deduster 
 dust from storage piles, wet sludge from 
 
Geology — 1940 Meeting 
 
 Fig. 3 (above). — Coal particles 35 x 48 mesh; 
 a. fusain; b. vitrain 
 
 Fig. 6 (below). — Fusain in thin section. 
 
 washeries, dry sludge from settling 
 basins, -% inch screenings of washed 
 coal, and raw carbon from storage piles 
 and loading docks. 
 
 Method of Study. In making a petro- 
 graphic determination of fusain, approx- 
 imately 500 grams of the fine coal to be 
 studied were cut from the mine sample 
 with a Jones-type riffle. The riffle sample 
 was weighed and screened through a bat- 
 tery of Tyler standard screens having 
 openings in the fixed ratio of the square 
 root of two. The battery of screens was 
 divided into two nests from 4 (4.7mm) 
 mesh to 35 (.417mm) mesh and from 
 48 (.295mm) mesh to 300 (.046mm) 
 mesh. The first set of screens was 
 shaken in a Ro-Tap shaker for ten 
 minutes and the second set containing 
 the finer screens for fifteen minutes. The 
 material retained on each screen was 
 weighed and placed in a marked con- 
 tainer. 
 
 The essential purpose of screening was 
 to facilitate counting of the coal particles 
 by sorting the material into fractions hav- 
 ing a small size range. An ore-dressing 
 type binocular microscope was used in 
 identifying the coal particles. Fusain 
 particles were separated from the non- 
 fusain, and an accurate count of the two 
 classes of material was made during the 
 process of separation. 
 
 In the calculations it was assumed that 
 the percentage of fusain by microscopic 
 count also represented weight per cent, 
 that is that all coal particles on any 
 one screen are of the same volume and 
 specific gravity. The validity of these 
 assumptions was tested by manually 
 separating the fusain from non-fusain on 
 seventeen screens and determining the 
 actual percentage of each class by weight 
 and by count. The average fusain con- 
 tent of these samples was 2.67 per cent by 
 weight and 2.65 per cent by count. 
 
 Coal research workers in Europe and 
 in the United States, particularly at Penn- 
 sylvania State College Experiment Sta- 
 tion, have developed the Fuchs method 3 
 of fusain determination which consists of 
 treating the coal sample with nitric acid 
 to oxidize the non-fusain which is then 
 removed by solution with sodium hy- 
 droxide. The unoxidized fusain residue 
 is ashed and the fusain percentage is cal- 
 
8 
 
 Illinois State Academy of Science Transactions 
 
 culated from difference in weight. The 
 chemical method indicates that the ma- 
 terial passing the 300-mesh screen is pre- 
 dominately fusain and mineral matter. 
 In fusain containing no visible mineral 
 matter the Fuchs method may indicate as 
 much as 15 per cent inherent mineral 
 matter. Since it is impossible to count 
 fusain in the minus 300-mesh because of 
 the extreme variation in particle size, the 
 Fuchs method was used to determine it 
 in this fraction. 
 
 Results. The results obtained from siz- 
 ing the fractions and calculating the 
 fusain percentage of each size have given 
 important incidental information in re- 
 
 gard to the variation in friability of 
 fusain. It is generally recognized that 
 fusain concentrates in the finer sizes of 
 coal. It is also understood that fusain 
 possesses different degrees of hardness. 
 Some workers have used the terms 
 "hard" fusain and "soft" fusain. 
 
 The authors have prepared a series of 
 curves (Fig. 5) in which the percentage 
 of fusain in the material on each screen 
 was directly plotted on graph paper and 
 a curve drawn through the points. These 
 curves show graphically the tendency of 
 fusain toward concentration in the (finer 
 sizes. The lower part of the curves show 
 a gradual increase in fusain from screen 
 
 80 
 
 FUSAIN PERCENT (DIRECT PLOT) 
 
 Fig. 5 
 
Geology — 19J+0 Meeting 
 
 to screen in the coarser sizes up to 100- 
 mesh. In the sizes finer than 100-mesh 
 the fusain increases very rapidly and the 
 curves consequently take an abrupt rise 
 at this point. The flatness of the curves 
 in their lower portion is indicative of the 
 presence of fusain of a less friable type. 
 This fusain owes its hardness to minerali- 
 zation of characteristic pore spaces rep- 
 resenting the original cell lumens (Fig. 6). 
 The fusain percentage curves for de- 
 duster dust, sludge, washed coal screen- 
 ings, raw carbon, and whole coal samples 
 are very similar, although there is con- 
 siderable range in the total fusain con- 
 tent of these various types. The fusain 
 in washed coal screenings was as low as 
 four per cent and as high as 20 per cent 
 in deduster dust. The fusain content of a 
 
 whole coal sample cut from the face in a 
 Franklin County mine was 4.9 per cent. 
 A sample of raw carbon from the tipple 
 of the same mine contained 12.07 per cent 
 fusain. This relationship indicates that 
 the fusain of the whole coal is concen- 
 trated in the minus %-inch which repre- 
 sents about V 3 of the total production of 
 the mine. 
 
 The quantity of fusain in prepared or 
 sized Illinois coal greater than %-inch 
 is probably negligible. In the fine sizes 
 of coal resulting from natural breakage 
 and from preparation there is a relatively 
 low but gradually increasing percentage 
 of fusain in sizes above 100-mesh. In 
 sizes smaller than 100-mesh fusain in- 
 creases very rapidly reaching a maximum 
 percentage in the minus 300-mesh size. 
 
 1 111. Geol. Survey, Bull. 64, 116 and 150, 1937. 
 
 2 Personal communication. 
 
 3 Fuchs, W., et al., Penn. State College Bull. 23, 1938. 
 
 PRE-GLACIAL RIVER TICONA 
 
 H. B. WlLLMAN 
 
 State Geological Survey, Vroana, Illinois 
 
 The topography of north-central Illinois 
 reflects the glacial history of the area 
 and consists of a youthful surface with 
 the characteristic forms of glacial deposi- 
 tion locally modified by stream erosion. 
 Study of the topography of the bedrock 
 surface in outcrops and in records of 
 borings shows that the glacial deposits 
 conceal a drainage system strikingly dif- 
 ferent from the present drainage system. 
 The bedrock surface consists of a broad 
 gently-sloping surface, above which rise 
 elevations 40-50 feet high and in which 
 are eroded many deep branching valleys. 
 The general picture is that of a dissected 
 peneplain in late youth or early maturity. 
 
 The area studied centers about the 
 upper Illinois Valley (fig. 1) and in- 
 cludes most of LaSalle, Kendall, Will, 
 Grundy, Livingston, and Putnam counties. 
 The bedrock surface in this area was 
 drained westward, as at present, by a 
 river named River Ticona for the railroad 
 station of Ticona, which is located along 
 the buried valley a mile northeast of 
 Tonica. 
 
 Along the Ticona drainage divide the 
 pre-glacial upland surface generally has 
 
 an elevation of 600-625 feet, with some 
 hills as high as 650 feet, and locally near 
 Lisbon and Fairbury as high as 675 feet. 
 The upland surface has an elevation of 
 about 625 feet along the axis of the 
 LaSalle anticline near the west side of 
 the drainage area, and an upland level of 
 600 feet is common as far east as Mar- 
 seilles. Farther east the surface lowers 
 and is generally 525-550 feet in the 
 eastern part of the drainage area, 
 although it rises to the higher areas along 
 the drainage divide. The general slope of 
 the surface, therefore, is east, although 
 the main drainage is westward. 
 
 River Ticona occupied a valley both 
 broader and deeper than that of the 
 present Illinois River in the same area. 
 In the lower part of its course River 
 Ticona was entrenched in a steep-walled 
 valley at least 300 feet deep and about 
 1% miles wide at the top. The valley- 
 walls are exposed southeast of Lowell 
 where Vermilion Valley crosses Ticona 
 Valley almost at right angles. The bed- 
 rock surface lowers from near the top to 
 the bottom of the Vermilion valley-walls, 
 about 80 feet, in less than 100 yards. 
 
10 
 
 Illinois State Academy of Science Transactions 
 
 INOIS STATE GEOLOGICAL Si/Mlt 
 
 Fig. 1 
 
 Only the upper walls of Ticona Valley are 
 exposed, as its bottom is far below the 
 level of Vermilion River. At its mouth 
 the elevation of River Ticona was as low 
 as 300 feet, which is 150 feet below the 
 level of Illinois River. Although Ticona 
 Valley was eroded about 300 feet deep in 
 bedrock, the present Illinois valley, 
 locally 200 feet deep, has a maximum 
 depth in bedrock of only 175 feet. 
 
 Although the course of the main valley 
 of River Ticona is westward or directly 
 contrary to the general slope of the bed- 
 rock surface, the tributary valleys mostly 
 conform to the regional slopes. North of 
 Ottawa and at Streator the tributary 
 rivers flowed eastward away from the 
 high area along the axis of the LaSalle 
 anticline. The tributary river north of 
 Ottawa flowed eastward nearly 25 miles 
 before it joined Ticona River. In the 
 eastern half of the drainage area the 
 directions of the streams were more 
 
 normal, leading directly away from the 
 drainage divides. 
 
 In the erosion of an anticlinal area 
 such as the LaSalle anticline, a relatively 
 high area would normally remain along 
 the axis of the structure and thus form 
 a divide between divergent drainage sys- 
 tems. Such a high area occurs along the 
 LaSalle anticline, but peculiarly enough 
 the main drainage line of the area di- 
 rectly crosses it. It is of interest, there- 
 fore, to consider some of the events in the 
 history of the area which may have re- 
 sulted in the establishment of River 
 Ticona across the anticline. 
 
 Ticona valley contains glacial deposits 
 which have been correlated with the 
 Kansan stage of glaciation, and it was 
 therefore eroded before Kansan time. As 
 the youngest bedrock cut by the valley 
 is Pennsylvanian in age, the drainage 
 system is younger than the Pennsyl- 
 vanian deposits. On the basis of these 
 
 
Geology — 19J/0 Meeting 
 
 11 
 
 data alone, it might be logically assumed 
 that the position of Ticona valley across 
 the LaSalle anticline indicates the valley 
 is antecedent and was present before the 
 folding of the anticline in Late Paleozoic 
 time. Because of the great length of time 
 since the Paleozoic era, and the varied 
 history of the area as indicated by evi- 
 dence in other areas, it seems unlikely 
 that the drainage system of Late Pale- 
 ozoic time persisted to the Pleistocene 
 period. 
 
 Following the folding of the LaSalle 
 anticline at the end of the Paleozoic era 
 the area was eroded to a relatively flat 
 plain. Probably it was reelevated and 
 eroded again several times during the 
 Mesozoic and Cenozoic eras, and at least 
 600 feet of Paleozoic strata were eroded 
 from the area. It is possible that many 
 later strata, of which no remnants are 
 now present, may have been deposited 
 and also eroded. The area was probably 
 eroded to a peneplain during the early 
 Mesozoic time as the Cretaceous deposits 
 of the Gulf coast embayment overlie the 
 peneplaned surface of the older strata. 
 During Tertiary time the area was again 
 peneplaned, and the present upland sur- 
 faces of the bedrock are remnants of this 
 peneplain. The peneplain truncates the 
 LaSalle anticline and all the formations 
 from the Shakopee dolomite to the 
 youngest Pennsylvanian beds in less than 
 two miles, and in spite of their striking 
 differences in resistance to erosion, re- 
 tains a comparatively flat surface. Ero- 
 sional surfaces in the unglaciated area in 
 northwestern Illinois and southwestern 
 Wisconsin have been variously described 
 as the result simply of differential ero- 
 sion, or of one or two periods of pene- 
 planation subsequently modified by re- 
 juvenated erosion. A recent study 1 of 
 the problem has indicated that the high- 
 est upland surfaces are broad remnants 
 of a late Tertiary peneplain, named the 
 Dodgeville peneplain, and the slope and 
 elevation of the peneplain indicates its 
 identity with the one recognized in this 
 area. 
 
 Although the divide along the axis of 
 the anticline might be expected to per- 
 sist throughout the interval of pene- 
 planation, drainage might have been 
 established across the natural divides of 
 the surface during the uplift of the pene- 
 plain especially if accompanied by slight 
 warping of the surface. 
 
 It is also possible that sometime during 
 the Mesozoic era or Tertiary periods flat- 
 lying deposits were laid down across the 
 structure. If this happened a new drain- 
 age would be established dependent on 
 the slope of the surface of these beds 
 and regardless of the underlying struc- 
 ture. With erosion through these beds 
 the drainage would be superimposed on 
 the structure. The course of the major 
 river might persist across the anticline 
 but the courses of the tributaries might 
 be altered to follow the regional slopes 
 of the old buried surface, and new 
 streams developing would likely follow 
 the same slopes. Although this inter- 
 pretation adequately accounts for the 
 drainage pattern, it requires the deposi- 
 tion of beds which have since been com- 
 pletely eroded and it therefore cannot be 
 confirmed. 
 
 In late Tertiary time the area was 
 eroded to the level of the Dodgeville 
 peneplain, and the fact that the surface 
 of the peneplain is slightly higher along 
 the axis of the anticline suggests that 
 drainage was not established across the 
 anticline during the erosion of the pene- 
 plain. If River Ticona did not extend 
 across the anticline during erosion to 
 the level of the peneplain, it at least 
 took this position on the peneplain be- 
 fore uplift caused entrenchment of the 
 river in the peneplain. Because Ne- 
 braskan glacial deposits occur on the 
 peneplain and not in the valleys, it has 
 been suggested 2 that dissection of the 
 peneplain did not occur until after Ne- 
 braskan glaciation but before Kansan 
 glaciation. Therefore the course of River 
 Ticona may have been established during 
 the Nebraskan glaciation. 
 
 There is no direct evidence that the 
 Nebraskan ice invaded the Ticona drain- 
 age area. The nearest deposits correlated 
 with the Nebraskan glacier which ad- 
 vanced from the Keewatin center occur 
 in the northeastern corner of Iowa and 
 in west-central Illinois. However, the ice 
 may have extended farther east and, if 
 so, it might well have established new 
 drainage lines across the pre-existing 
 divides. It is also possible that a Nebras- 
 kan advance from the Labradorean center 
 blocked drainage eastward from the anti- 
 cline and forced an outlet westward over 
 the divide along the anticline. Any 
 Nebraskan deposits not eroded during 
 the dissection of the peneplain before the 
 
12 
 
 Illinois State Academy of Science Transactions 
 
 Kansan glaciation would be in the most 
 favorable place for erosion by the suc- 
 ceeding glaciers. In the Ticona basin 
 the Kansan, Illinoian, and earliest Wis- 
 consin deposits are found in Ticona val- 
 ley and its tributaries, and the later Wis- 
 consin deposits usually rest directly on 
 the bedrock on remnants of the pene- 
 plain. There may be, therefore, in the 
 discordant drainage pattern of the bed- 
 rock surface some evidence of Nebras- 
 kan glaciation not found in the glacial 
 deposits of the area. 
 
 In summary, the position of River 
 Ticona across the LaSalle anticline was 
 attained in the interval between the 
 Pennsylvanian period and the Kansan 
 age of the Pleistocene period. It might 
 be antecedent on the structure and late 
 Paleozoic in age; it could have been at- 
 
 tained during the uplift of the pene- 
 plains eroded during Mesozoic and Ter- 
 tiary time; it might have been superim- 
 posed on the structure during the same 
 interval; and it might be the result of 
 Nebraskan glaciation. Of these the latter 
 seems most likely. 
 
 Ticona Valley was gradually filled with 
 deposits during the succeeding glaciations 
 but it controlled the main drainage of 
 the area through Kansan, Illinoian, and 
 early Wisconsin time. The valley may 
 have been obliterated by the Blooming- 
 ton drift, and it certainly was by the 
 Cropsey drift, as the Inner Cropsey 
 moraine shows no depression where it 
 crosses the valley, and by that time 
 drainage was established along the pres- 
 ent course of Illinois Valley. 
 
 1 Bates. R. E., Geomorphic history of the Kickapoo region, Wis., Geol. Soc. Am. Bull, 
 vol. 50. 1939, pp. 819-880. 
 
 2 Trowbridge, A. C, The erosional history of the Driftless Area, Univ. of Iowa Studies 
 in Nat. Hist., vol. 9, No. 3, 1921. 
 
Geology — 19JfO Meeting 
 
 13 
 
 AERIAL PHOTOGRAPHY 
 
 Harry McDermith 
 Urbana, Illinois 
 
 Photographing from the air on a large 
 or commercial scale is a comparatively 
 new industry. However, since the air- 
 planes came into use, and especially since 
 the start of the great World War, aerial 
 photography has become very popular. 
 The first photographs of this type date 
 back to about 1865. With a few limited 
 exceptions, this work previous to 1914 
 was done from kites, balloons and 
 dirigibles. Kites and balloons were un- 
 satisfactory in that they were at the 
 mercy of the winds, making it impractical 
 to carry out accurate and systematic 
 photographic plans. The dirigible is quite 
 satisfactory insofar as stability, room for 
 operation and speed of motion is con- 
 cerned; however, it is too expensive to 
 operate. The airplane has now proven 
 itself to be the most practical and eco- 
 nomical of all air transports for aerial 
 photographing. 
 
 Commercial and army airplanes are 
 most commonly used in this work. The 
 Fairchild "71", Lockheed, and the Cessna 
 have been among those extensively used 
 in this country. There has not been a 
 plane constructed yet that possesses all 
 the qualities desired in a photographing 
 ship. However, an attempt has been made 
 to construct such a plane by the Abrams 
 Aircraft Corporation of Lansing, Michi- 
 gan, in building what they call the 
 "Explorer". This is a pusher-type single- 
 motored monoplane with the cockpit 
 enclosed with plexiglass or a similar 
 material. The following features of spe- 
 cial importance are included in this 
 plane: wide radius of visibility, rapid 
 climbing ability, high cruising speed, 
 stability, and the camera is placed ahead 
 of the motor. 
 
 Photographing from the air was carried 
 on in a very limited scale until the be- 
 ginning of the World War. Then when 
 it was found that these photographs could 
 be so effectively used in reconnaissance 
 surveys over the enemy lines in deter- 
 mining the position, size and direction of 
 motion of troops as well as in furnishing 
 
 a fine planimetric map of the country, 
 aerial photography took a big jump. By 
 the end of the war the aerial mapping 
 units in all government armies had been 
 enlarged considerably. This revolution- 
 ized military operation completely. After 
 the war, activity in this field was car- 
 ried on by the U. S. Geological Survey, 
 the U. S. Coast and Geodetic Survey, and 
 the U. S. Army Engineers on a rather 
 small scale for mapping and planning work. 
 In 1935 the Agricultural Adjustment Ad- 
 ministration, under the U. S. Department 
 of Agriculture, started a systematic and 
 extensive plan of aerially photographing 
 this country. The primary purpose was 
 for the administration of the crop-control 
 program. This department has photo- 
 graphed approximately 2,000,000 square 
 miles in this country at an estimated cost 
 of $6,900,000 in the last ten years, of 
 which 90 per cent has been performed 
 since 1934. Aerial photographic operation 
 under the AAA began in this State in 
 1936 when eleven counties were photo- 
 graphed. The original photography for 
 the entire State was completed in the fall 
 of 1939. 
 
 The photography by the AAA is per- 
 formed with a single-lens, high-precision 
 aerial photographing camera mounted in 
 a vertical position. The pictures are 
 taken at an altitude of 13,500 to 17,000 
 feet, with each picture overlapping the 
 preceding one about 60 per cent, and 
 those in adjacent flight strips 30 per cent. 
 The size of the negatives are 7" x 7" and 
 7" x 9", covering respectively approxi- 
 mately 6 and 7 square miles, depending 
 upon height of plane at time of exposure. 
 At this height and using a camera having 
 an 8*4" focal length the scale of these 
 negatives are 1:20,000, or approximately 
 1" = 1,700 feet. Oblique and vertical pho- 
 tographs using a multiple lens camera 
 have been used extensively in Canada, 
 Alaska, and several European countries. 
 
 The bureaus of the various govern- 
 mental departments that are making ex- 
 
14 
 
 Illinois State Academy of Science Transactions 
 
 tensive use of aerial photographs are as 
 follows: Department of the Interior — the 
 U. S. Geological Survey, General Land 
 Office, and Bureau of Biological Survey; 
 Department of Commerce — U. S. Coast 
 and Geodetic Survey; Navy Department — 
 Hydrographic Office; War Department — 
 Corps of Engineers; Federal Works 
 Agency — Public Works Administration; 
 Department of Agriculture — AAA, Forest 
 Service, Soil Conservation Service, and 
 Bureau of Plant Industry. Other federal 
 agencies are Tennessee Valley Authority, 
 Mississippi River Commission, Interna- 
 tional Boundary Commission, Lake Sur- 
 veys, Post Office Department, National 
 Park Service, Rural Electrification, and 
 Department of Justice. 
 
 It is impossible in this paper to 
 enumerate and elaborate on all the pos- 
 sible uses of aerial photographs; how- 
 ever, some of the more interesting uses 
 
 are listed below: a. making of plans for 
 auxiliary landing fields; b. studies for 
 dam construction and reservoirs; c. drain- 
 age regulation and canal projects; d. 
 planning and erecting communication 
 lines; e. topographic and planimetric 
 mapping; f. crop control and soil preser- 
 vation; g. illustrations for tourists and 
 passenger guidebooks; h. study of posi- 
 tion and shape of natural boundary lines, 
 mountain ranges, rivers, streams, and 
 timber; i. studying and tracing bedrock 
 outcrops, faults, limestone sinkholes, 
 landslides, underground and surface water 
 courses; j. mapping and studying of oil 
 and coal field activities; k. military 
 operation. 
 
 In conclusion, I wish to state that the 
 principal concern of this paper is to 
 bring to your attention the endless uses 
 that can be made of airplane photographs 
 in both private and governmental work. 
 
Geology — 1940 Meeting 
 
 15 
 
 THE USE OF PIPETTE ANALYSIS IN CLAY RESEARCH 
 
 Richards A. Rowland* 
 State Geological Survey, Vrbana, Illinois 
 
 One of the methods used in the study 
 of clays is the determination of the dis- 
 tribution of the particle sizes of both clay 
 and non-clay mineral material. Of the 
 several means available, pipette analysis 
 is the most useful, because in addition 
 to comparative size data, a sample is ob- 
 tained from which a microscopic exam- 
 ination can be made to determine the 
 abundance of each constituent in each 
 size. 
 
 There is a tremendous variation in the 
 size distribution of clays and a definite 
 lower limit at which ordinary mechanical 
 analyses will give reproducible results. 
 The smallest screen size through which 
 a clay may be wet-screened in a reason- 
 able length of time is the No. 270, the 
 openings of which are about 53 microns. 
 The largest size particle for which pipette 
 analysis will give consistent results is 
 about 20 microns. A critical cross-sec- 
 tion of a clay is obtained by spacing the 
 pipette fractions at 20, 10, 5, 2, 1, and 
 0.5 microns. When used with the 270 
 mesh screen, these sizes make a very 
 even spread of data on three cycle semi- 
 log paper for either a cumulative or dis- 
 tribution curve. They include the range 
 of clay material (less than 20 microns) set 
 by the American Foundrymen's Associa- 
 tion for the study of bonding clays, the 
 U. S. Bureau of Soils upper limit of clay 
 (five microns) and the size (two mi- 
 crons) below which most clay investiga- 
 tors agree that a clay material is pre- 
 dominantly clay mineral. 
 
 These sizes lend themselves to a simpli- 
 fied plotting of Stokes' law because the 
 relation between each diameter is a whole 
 number. Stokes' law, V = 2aR 2 (Di-D), 
 
 9v 
 where a = acceleration due to gravity; 
 R = radius of particle; Di = Sp. G. of 
 particle; D = Sp. G. of water at temp, 
 used; v = viscosity of water at temp. 
 
 used; V = time to fall 1 cm.; for any 
 one temperature may be reduced to V = 
 KR 2 where K is a constant K = 
 (2a(D 1 -D) 
 
 9v 
 
 At any one temperature, therefore, the 
 sizes chosen have settling velocities 
 which are multiples of each other. For 
 example, the velocity varying as the 
 square of the radius, for a particle of 
 20 microns diameter, R 2 = 100, and for a 
 particle of 10 microns R 2 = 25. The ratio 
 of the velocities is 4 to 1 or the 20 
 micron particle settles 4 times as fast as 
 the 10 micron particle. Likewise, the 
 0.5 micron settling time is 4 times that 
 of 1 micron, 16 times that of 2 microns, 
 2 microns is 100 times that of 20 microns, 
 0.5 microns is 100 times that of 5 microns 
 and 1 micron is 100 times that of 10 
 microns. 
 
 The graph (fig. 1) was plotted from 
 data computed at 15, 20, 25 and 30 de- 
 grees Centigrade for particles 20, 10, 5, 
 2, 1, and 0.5 microns in diameter assum- 
 ing an effective specific gravity of 2.65. 
 Points were first plotted for 0.5 micron 
 using the smallest unit of the paper 
 (1/20 inch) as one minute. The scales 
 for each of the other sizes were then 
 computed to fit the curve drawn through 
 the 0.5 micron points. The following 
 table gives values for both the large and 
 small units of the scale for each particle 
 size. 
 
 To obtain the settling time for any of 
 the sizes 20, 10, 5, 2, 1, and 0.5 microns, 
 choose in the left column the temperature 
 best suited to the room or bath in which 
 the analysis is to be made. Follow the 
 horizontal line on which this temperature 
 lies until the heavy black line of the 
 graph is reached. Then the vertical line 
 which passes through the graph at this 
 point marks the time required for each 
 particle to settle 1 cm. on each of the 
 scales. 
 
 * Assistant petrographer, Illinois State Geological Survey. 
 
16 
 
 Illinois State Academy of Science Transactions 
 
 !_Ih-J - !'"H ! . .| ■.;... | ..;. ! | :.. ; ...J '~ 
 
 ' ' PF ;^ A ^ u :^hU":^ c l^ r > 7AVITY - l 2e5 :-- frrTrftfffl 
 
 s ■ r ■■:.', 
 
 Fig. 1. 
 
 Diameter 
 of 
 
 Large 
 
 Small 
 
 particle 
 
 units 
 
 units 
 
 0.5 
 
 10 min. 
 
 60 sec. 
 
 1.0 
 
 2.5 min. 
 
 15 sec. 
 
 2.0 
 
 0.625 min. 
 
 3.75 sec. 
 
 5.0 
 
 6 sec. 
 
 0.6 sec. 
 
 10.0 
 
 1.5 sec. 
 
 0.15 sec. 
 
 20.0 
 
 0.375 sec. 
 
 0.0375 se 
 
 Taele 1 
 
 Diam. of 
 
 Time to settle 
 
 Depth of 
 
 Time of 
 
 particle 
 
 1 cm. at 25°C. 
 
 settling 
 
 settling 
 
 0.5 
 
 11° 2'15" 
 
 2 cm. 
 
 22° 4'30" 
 
 1.0 
 
 2°45'30" 
 
 2 cm. 
 
 5°31'00" 
 
 2.0 
 
 41'23" 
 
 5 cm. 
 
 3°26'55" 
 
 5.0 
 
 6'37" 
 
 10 cm. 
 
 1° 6'10" 
 
 10.0 
 
 1'39" 
 
 10 cm. 
 
 16'30" 
 
 20.0 
 
 24.8" 
 
 10 cm. 
 
 4' 8" 
 
 In practice the most suitable times for 
 each particle size have been controlled by 
 immersing the pipette to different depths 
 (table 1). In this fashion, a complete 
 analysis of all particle sizes may be 
 finished in 24 hours, or thereabouts. By 
 contrast, the usual hydrometer analysis 
 in 24 hours would furnish data only to 
 about 2 microns. A constant temperature 
 bath agitated by bubbling air, not strong 
 enough to shake the cylinders but enough 
 to circulate the water, and controlled by 
 a mercury temperature control attached 
 to a switch tube which turns on and off 
 a knife type electric heater will give re- 
 sults reproducible to one tenth of a per- 
 cent on duplicates from the same sam- 
 ple. The most usual temperature is 
 25° C. Table I has been computed from 
 fig. 1. 
 
 In interpreting pipette analysis of clays 
 it cannot be too strongly emphasized that 
 
 the data represents only the degree to 
 which it has been disaggregated and that 
 it is impossible to completely break up 
 the aggregates of a clay. In addition the 
 particle diameters for each size meas- 
 ured are only equivalent sizes, that is 
 they represent a particle, the mass and 
 surface area of which cause it to settle 
 at a rate equivalent to the rate at which 
 a sphere of the same effective mass might 
 settle. 
 
 If these two objections are taken into 
 account and a good suspension is ob- 
 tained beforehand, the data from pipette 
 analyses will serve to compare clays 
 which have been subjected to an identical 
 preparation. 
 
 By using different means of disaggre- 
 gation it is possible to obtain large 
 variations in the size analyses of the 
 same clay. 
 
Chemistry — 19JfO Meeting 
 
 17 
 
 THE INTRODUCTION OF FLUORINE INTO AROMATIC 
 NUCLEI BY MEANS OF AMMONIUM FLUOBORATE 
 
 G. C. Finger and F. H. Reed 
 State Geological Survey, Vroana, Illinois 
 
 Fluorine is most conveniently intro- 
 duced into the aromatic nucleus by means 
 of the diazonium fluoborate synthesis dis- 
 covered by Bart 1 , and developed by Schie- 
 mann 2 . In brief, the reaction involves the 
 diazotization of an aromatic amine, con- 
 version to the insoluble diazonium fluo- 
 borate, and subsequent thermal decompo- 
 sition to the aromatic fluoride. It is il- 
 lustrated as follows: 
 
 ArNH 2 * -> ArN 2 + -> ArN,BF 4 
 -> ArF + N 2 + BF 3 
 The diazonium fluoborates in a relatively 
 pure state have characteristic and defi- 
 nite decomposition temperatures below 
 which they are stable, and, in many 
 cases, can be stored for indefinite periods 
 of time. 
 
 Fluoboric acid was originally used to 
 form the diazonium salt. The resulting 
 acid medium was exceedingly corrosive to 
 glass or metal equipment. Due to the 
 commercial significance of this reaction, 
 it was improved upon by the use of sod- 
 ium fluoborate 3 - 4 thus avoiding the use 
 of corrosive hydrofluoric and fluoboric 
 acids. This improvement has made it 
 possible to prepare many aromatic flu- 
 orine compounds in the laboratory at a 
 reasonable cost in ordinary glass ap- 
 paratus. 
 
 Ammonium fluoborate has become avail- 
 able and can be prepared in a much purer 
 form on an industrial scale than the 
 sodium salt due to its lower solubility. 
 This study was made to determine 
 whether ammonium fluoborate can be 
 used in place of the sodium salt. 
 
 Aniline, o-toluidine, a-naphthylamine, 
 and benzidine were converted to the cor- 
 responding diazonium chlorides. Each 
 diazonium chloride solution was then di- 
 vided into two equal portions, one was 
 treated with a calculated excess of sodium 
 fluoborate, and the other with an equal 
 excess of ammonium fluoborate. Since 
 the ammonium salt is less soluble than 
 the sodium salt its molar solution volume 
 was larger. Each precipitate pair was 
 then filtered, washed, dried, and weighed 
 in the usual manner under identical con- 
 ditions. The results are semi-quanti- 
 tative in nature and are based on the dia- 
 zonium fluoborates. The data in this 
 form are interesting not only from the 
 standpoint that the diazonium fluoborates 
 can be used to form dyes 5 but the -N 2 BF 4 
 group can be replaced by acetoxy 6 , mer- 
 cury 7 , nitro 8 , and arsonic acid 9 groups. 
 Thermal decomposition in all cases gave 
 the corresponding nucleated fluorine com- 
 pound. 
 
 Table I.— Yield of Aryl Diazonium Fluoborates With Sodium Fluoborate and Ammonium Fluoborate 
 
 
 Moles 
 
 of 
 Amine 
 
 Moles 
 
 of 
 MBF4 
 
 NaBF 4 
 
 
 NH4BF4 
 
 
 Amine 
 
 Grams of 
 ArN 2 BF 4 
 
 Yield 
 in% 
 
 Avg. 
 % 
 
 Grams of 
 ArN 2 BF 4 
 
 Yield 
 in% 
 
 Avg. 
 
 Aniline 
 
 0.25 
 0.5 
 
 0.25 
 0.5 
 
 0.25 
 0.25 
 
 0.15 
 0.15 
 
 0.3 
 0.6 
 
 0.3 
 0.6 
 
 0.3 
 0.3 
 
 0.34 
 0.34 
 
 33 
 69.5 
 
 31 
 59.5 
 
 40 
 45 
 
 49 
 47 
 
 69 
 72.5 
 
 60 
 58.8 
 
 66 
 73 
 
 85 
 82 
 
 70.7 
 59.4 
 69.5 
 83.5 
 
 28 
 56 
 
 34 
 54 
 
 37.5 
 
 47.7 
 
 43 
 53.5 
 
 58 
 58 
 
 65 
 52.5 
 
 62 
 
 78 
 
 75 
 93 
 
 
 o-Toluidine 
 
 58 
 
 
 58.7 
 
 Benzidine 
 
 70 
 
 
 84 
 
18 
 
 Illinois State Academy of Science Transactions 
 
 The data in Table I indicate that the 
 ammonium salt gives .yields as satisfac- 
 tory as the sodium salt except with ani- 
 line. Since the solubility of the diazon- 
 ium fluoborate is an important factor, the 
 decreased yield in the case of aniline may 
 be due to the larger volume necessary 
 with the ammonium salt. 
 
 Since this study is preliminary in na- 
 ture, other amines will be studied as well 
 as some of the factors involved. The 
 authors wish to express their appreciation 
 to the Aluminum Ore Co. of East St. 
 Louis for furnishing the commercial sam- 
 ples of the sodium and ammonium fluo- 
 borates. 
 
 Conclusions. — Ammonium fluoborate can 
 be used satisfactorily in the preparation 
 
 * Ar represents an aromatic radical. 
 
 of some aromatic fluorine compounds by 
 means of the Schiemann reaction. 
 
 Bibliography 
 
 1. Bart, Ger. patent 281,055 (Oct. 12, 1914). 
 
 2. Balz and Schiemann, Ber. 60, 1186 (1927). 
 
 3. LeFevre and Turner, J. Chem. Soc. 19 SO, 
 1158. 
 
 4. Meigs, U. S. patent 1,916,327 (July 4, 
 1933). 
 
 5. Ruggli and Casper, Helv. Chim. Act. 18, 
 1414 (1935). 
 
 6. Haller and Schaffer, J. Am. Chem. Soc. 
 55, 4954 (1933). 
 
 7. Dunker, Starkey and Jenkins, ibid. 58, 
 2308 (1936). 
 
 8. Starkey, ibid. 59, 1479 (1937). 
 
 9. Ruddy, Starkey and Hartung, unpub- 
 lished results. 
 
 2-CHLORO-3,5-BIS ( ACET YLAMINO ) TOLUENE 
 
 G. R. Yohe 
 
 Illinois State Geological Survey, TJroana 
 
 Incidental to the identification of o-chlor- 
 otoluene in a reaction mixture, 2-chloro- 
 3,5-bis ( acetylamino ) toluene was pre- 
 pared. This compound is mentioned in 
 the literature 1 . 2 but its constants 
 apparently have not been published. It 
 was prepared by nitration of the fraction 
 to be identified, reduction with tin and 
 hydrochloric acid, and acetylation of the 
 amine with acetic anhydride. Mixed melt- 
 ing point determinations showed it to be 
 identical with the product prepared from 
 authentic o-chlorotoluene by the following 
 reactions: 
 
 Nitration of o-chlorotoluene with 
 HNO3-H2SO4 yielded a semisolid product 
 from which 2-chloro-3,5-dinitrotoluene, 
 m. 62-3° (cor.) was isolated by repeated 
 recrystallization from carbon tetrachlo- 
 ride. Previously recorded melting points 
 are 63-4 ° 3 , 65 ° 4 and 45 °i. The last value 
 
 is incorrect. 
 
 The dinitro compound was reduced with 
 tin and hydrochloric acid to 2-chloro-3, 
 5-diaminotoluene which, after recrystalli- 
 zation from water, melted at 72-3° (cor.). 
 The literature gives 73 0l or 74 ° 2 . 
 
 The diamine was stirred with a slight 
 excess of acetic anhydride until crystals 
 formed; these were washed with cold 
 water and recrystallized from about 400 
 parts by weight of water. 2-chloro-3, 
 5-bis ( acetylamino ) toluene forms fine 
 white fibrous needles, m.p. 227-8° (cor.), 
 soluble in acetic acid, acetone and alcohol, 
 difficultly soluble in ether and benzene, 
 almost insoluble in hexane (60-70°) and 
 carbon tetrachloride. 
 
 The compound was analyzed by the 
 semi-micro Kjeldahl method by Mr. C. A. 
 Harman. Calcd. for CiiH 13 ClN 2 02: N, 
 11.64%. Found: 11.80, 11.58. 
 
 1 R. Nietzke and E. Rene. Ber. 25, 3005-9 (1892). 
 
 2 G. T. Morgan. J. Chem. Soc. 81, 86-100 (1902). 
 
 3 W. Borsche and A. Fiedler. Ber. 1,5, 270-3 (1912). 
 
 4 G. Korner and A. Contardi. Atti. accad. Lincei 24, I, 888-96 (1915). 
 
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