12 



Group of Scotland by Love (I960). He 

 found that small: spores in the nonmarine oil 

 shale are very similar in kind and relative 

 abundance to those in the nonmarine lime- 

 stone, but that a distinct change in propor- 

 tion of genera occurs in the marine Pumpher- 

 ston Bed. Staplin (1960, p. 1-3) reported 

 that in the Golata Formation (Mississippian); 

 of Canada the frequency distribution of spore 

 genera in the shale below the underclay, in 

 the underclay, and in the coal differs mark- 

 edly. The spore assemblage in the shale above 

 the coal is like that of the shale beneath the 

 underclay. 



Sullivan (1962), in his study of a West- 

 phalian sequence in South Wales, suggested 

 that the ranges of spore species in coal and 

 shale are quite similar. He noted that 

 changes in composition of spore assemblages 

 between coal and immediately overlying 

 shales were no greater than changes found 

 by Smith (1957) from one thin band of coal 

 to another. 



potassium hydroxide by several changes of 

 water. 



The cleared residue was sieved with a 65- 

 mesh Tyler screen, which has openings of 

 210 ft. The coarse residue remaining on the 

 screen was examined under a binocular mi- 

 croscope for megaspores. A small portion of 

 the fine residue was stained with safranin Y 

 for 3 hours to help make some spore struc- 

 tures more readily visible and to improve the 

 quality of the photomicrographs. The liquid 

 was decanted and, after dehydration by use 

 of 50 percent, 95 percent, and finally abso- 

 lute alcohol, the residue in a final solution of 

 50 percent xylol and 50 percent absolute 

 alcohol was mounted in liquid Canada bal- 

 sam. The slides were dried in an oven at 

 105° F for at least 5 days. Surplus residue 

 was stored in vials at the Illinois State Geo- 

 logical Survey. Opaque megaspores were 

 placed on pasteboard slides, and translucent 

 large spores and megaspores were mounted in 

 liquid Canada balsam after dehydration in 

 alcohol. 



PREPARATION 

 TECHNIQUES 



GOAL 



Plant microfossils were isolated from coal 

 samples by the standard maceration tech- 

 niques described in detail by Kosanke (1950, 

 p. 9-10). Core samples were cut on a car- 

 borundum saw to obtain a representative 

 sample of about 50 grams that would be small 

 enough to handle easily. Outcrop samples 

 were divided with a riffle into workable quan- 

 tities of about 50 grams. The coal was broken 

 into small fragments, placed in a beaker, and 

 covered with about 250 ml of Schulze's solu- 

 tion ( 1 part saturated solution of potassium 

 chlorate to 2 parts concentrated nitric acid) , 

 which partially oxidizes the coal. After about 

 3 days, the length of time depending upon the 

 ■composition of the coal, the residue was neu- 

 tralized by repeated washings, and 250 ml 

 of a 1 percent solution of potassium hydrox- 

 ide was added to dissolve the humic matter. 

 The residue was examined frequently in or- 

 der to determine the length of time required 

 for the appearance of an abundance of spores. 

 From 2 to 4 hours was required, after which 

 the undissolved plant material was freed of 



LIMESTONE, SILTSTONE, 

 SHALE, AND CLAY 



From each major lithology above and be- 

 low the coals, approximately 30-gram samples 

 were selected for maceration. All calcareous 

 samples were first placed in a 20 percent so- 

 lution of orthophosphoric acid until the lib- 

 eration of gas had ceased. After repeated 

 .washing to remove all the dissolved carbonate 

 minerals, hydrofluoric acid (reagent grade, 

 48 percent) was added to dissolve the silica 

 minerals present. Frequent stirring was nec- 

 essary to allow the acid to come into contact 

 with all the sludge. After about 16 hours, 

 water was added and decanted a number of 

 times until the sample was free of acid. Sev- 

 eral hard shale samples required an addi- 

 tional treatment of fresh hydrofluoric acid 

 for up to 16 hours. The remaining organic 

 matter was oxidized in Schulze's solution from 

 a few minutes to about 1 hour, cleared of 

 acid, then placed in a 10 percent solution of 

 potassium hydroxide for about 1 hour. Mi- 

 croscopic crystals of undetermined composi- 

 tion that formed after the potassium hydrox- 

 ide solution was added were dissolved by the 

 addition of a few drops of concentrated hy- 

 droehloric acid. 



