558 



Annals New York Academy of Sciences 



Blanks, rinses, Holbrook extracts, and 1-Murray 6- to 20-hour extract did not 

 absorb significantly in the 2 to 15 ^ infrared region. The infrared spectra of 

 the total blanks, and total Holbrook, l-()rgueil, and 2-Murray organic extracts 

 are presented in figure 1. In figure 2 are shown the spectra of the individual 

 chromatographic fractions of the 2-Orgueil extract. 



Ultraviolet and visual spectroscopy. All blanks, extracts, rinses, and chro- 

 matographic fractions were scanned in 220 to 400 ni/u region. Scans were run 

 on a Gary model 14 spectrometer with matched cells of 1 cm. in length and 

 methanol as solvent. Visual spectra were run on the benzene and methanol 

 chromatographic fractions of the 1-Orgueil, and 1-Murray. Absorption 

 decreased continuously from 400 to 800 m^ in all of these fractions. The 



Table 2 



Silica Gel Chromatographic Fractions 



(Weights in milligrams) 



1-Orgueil (6.0) 

 1 -Murray (1.1) 

 2-Murra'v (6.7) 

 Blank 



w-Heptane 



0.1 (0.3*) 

 0.0 (0.1*) 

 0.4 

 0.1 (0.0*) 



Carbon 

 tetrachloride 



0.2 

 0.1 

 0.1 

 0.0 



Benzene 



0.6 



0.0 (0.1*- 



0.4 



0.0 



t) 



Methanol 



4.4 

 0.7 

 4.3 

 0.1 (O.Ot) 



* Estimated from mass spectra peak heights. 

 t Estimated from ultraviolet absorption. 



Table 3 



Silica Gel Chromatographic Fractions of 2-Orgueil 



(Weights in Milligrams) 



I 



2-Orgueil aliquots 



Awt. 24.50 

 B wt. 25.09 

 C wt. 24.19 



Carbon 

 tetrachloride 



1.46 (6.0%) 

 1.32 (5.3%,) 

 1.17 (4.8%,) 



Benzene 



0.76 (3.\%) 

 0.82 (3.3'^) 

 0.76 (3.1%) 



Left on column 



4.96 (20.2%) 

 4.58 (18.3%) 

 4.08 (16.9%) 



Orgueil extracts ab.sorbed the strongest in the visual range, but the visual 

 spectra of all extracts lacked any suggestion of a specific absorption at a particu- 

 lar wavelength. 



The blanks did not absorb and the chromatographic fractions of the Holbrook 

 absorbed only slightly in the 220 to 400 niyu range. The ultraviolet spectra of 

 the 1-Orgueil and 2-Murray chromatographic fractions are presented in figures 

 3 and 4, respectively. In figure 5 are given the ultraviolet spectra of the 

 total Holbrook extract and the total procedure blank. The Murray and 

 Orgueil extracts fluoresced in ultraviolet light. 



Mass spectroscopy. Blanks and the rinse; 6-hour and 6- to 20-hour extracts 

 of Holbrook; and carbon tetrachloride, benzene, and methanol eluates of the 

 Orgueil distillate did not produce measurable peaks at masses greater than 150 

 in the mass spectrometer. Measurable mass spectra were obtained of the 4 

 individual chromatographic fractions of the 6-hour extract of 1-Orgueil and 



1 



