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July 9, 1946. ' ' C. B. BROWN METHOD FOR DETERMINING THE PETROLEUM HYDROCARBON2 403,631 , . CONTENT OF EARTH SAMPLES Filed July 5, 4 1943 9 Patented July 9, 1946 2,403,631 UNITED ‘STATES PATENT OFFICE‘ f 2,403,631 METHOD FOR DETERMINING THE PETROLE UM HYDROCARBON CONTENT OF EARTH SAMPLES Charles B. Brown, McAllen, Tex. Application July 5, 1943, Serial No.493,'60.6 3 Claims. (01. 250-833) 1 This invention relates to a method for use in tion. The ?uorescent light issuing from the locating oil deposits and oil bearing strata en countered in wells being drilled for oil and has portion '01’ the. solvent is passed, through a spectral :?lter, separated into its spectral compo nents, the intensity of each of which is deter more particular reference to an improved method for accurately analyzing earth samples for the mined petroleum hydrocarbon and pseudo-hydrocarbon content thereof. _ or measured . by any well, known photometric technique suitable for the purpose. The ?uorescent light issuing from each ' In the processes of exploration for petroleum and petroleum bearing strata by analysis of earth samples for their hydrocarbon content hereto hydrocarbon in solut'on possesses a spectral dis tribution individual thereto. The type and fore employed, considerable di?iculty has arisen 10 concentration of each hydrocarbonof the sample is determined by comparing the spectral compo in distinguishing between those hydrocarbons as nent intensity thereof with the aforesaid sociated with petroleum deposits and petroleum bearing strata and those hydrocarbons associated , ,, empirical charts until an empirical chart is found which possesses the same degree of ?uorescence with organic phenomona unrelated to petroleum 1 deposits and petroleum bearing strata. 'Attempts 15 as the hydrocarbon being measured. One of the objects of the invention is to provide have been made to use the ?uorescent phenom a new and improved method of separating and ena observed when hydrocarbons and their solu tions are subjected to ultraviolet radiation for the ; ' accurately measuring the concentrations of the various hydrocarbons and pseudo-hydrocarbons purpose of analysis, but this method has not been entirely satisfactory because of the interference 20 found in earth samples and of distinguishing between those hydrocarbons and pseudo of hydrocarbons not associated with petroleum hydrocarbons associated with petroleum and causing false indications. Furthermore, with the method heretofore employed, the intensity of ' - petroleum bearing strata and those hydrocarbons ?uorescence has been ‘found to be not directly 25 not associated with petroleum. and petroleum bearing strata. Another object is, to provide a proportional to the concentration of the various method of accomplishing the aforesaid object hydrocarbons in solution and for this reason rapidly in contradistinction to the relatively slow such methods do not afford an accurate measure of the hydrocarbon content of the earth sample. . > laboratory methods now in general use. _ v'I'he improved method in accordance with the 30 7 Still other objects and advantages will be apparent from they following description taken in present invention eliminates these difficulties by connection with the sheet of drawing on which is , preparing a series of standard empirical charts, _ shown in diagrammatic form the various ele separating each of the fluorescent effects of the ments and instrumentalities employed with my various hydrocarbons, and accurately measuring invention according to a preferred embodiment the concentration of each hydrocarbon by com-. thereof. parison of the separated ?uorescent e?ect thereof 35 Referring now to the drawing for a more with the empirical charts. The empirical'charts _ complete understanding of the invention, ultra may be conveniently prepared by using a series violet rays are radiated from a suitable source I of known hydrocarbons having known concen arranged within a hOusing 2 and passing through My method comprises the following steps: The 40 an opening 3 therein. A ?lter 4 is arranged within the path of travel of the ultraviolet rays earth sample to be analyzed is dried to remove to remove the visible components of the radia excess moisture and ground to approximately 100 tion whereby only the invisible radiation mesh ?neness using any well known‘ standard laboratory technique. A measured quantity of. component passes through the aperture 5 in the 45 shield 6. The intensity of the ultraviolet radia the sample is placed in a suitable‘vessel and a tion is controlled by passing it thru the predetermined quantity of a hydrocarbon solvent adjustable ultraviolet absorbing wedge shaped known to be non-?uorescent of itself is added member 1 having a plurality of graduated cali thereto. The mixture thus formed comprising brations 8 thereon. The ultraviolet radiation the sample and the solvent is allowed to settle trations. . thus controlled in intensity passed through the and a convenient measured portion of the solvent is transferred‘to a vessel composed of a material vessel 9 composed of a material which is trans parent to the ultraviolet radiation. The vessel 9 v transparent to ultraviolet radiation. The trans contains the solvent sample III which is caused parent vessel containing the measured portion of a he solvent is subjected to an ultraviolet radia 55 to ?uoresce when subjected to the ultraviolet radiation at II. The ?uorescent illumination 2,403,631 3 drocarbons of a measured quantity of an earth sample, subjecting a measured quantity of said solution to an ultraviolet radiation, passing the ?uorescent light emanating from said solution from that portion ll of the sample is passed through a spectral ?lter l2 and falls on a photocell 13. The photocell is connected in circuit with a calibrated meter M, battery B and switch $10. through a. plurality of spectral ?lters in succes , sion, each of said ?lters corresponding respective With the switch Sw moved to the closed position 1y to one of a plurality ‘of different bands of the spectrum, measuring the intensity of ?uorescent the intensity of the ?uorescent illumination at I3 is measured by comparingthe reading of the light in each one of said spectral bands respec meter M with a previously determined calibration 10 tively, and in comparing the measured intensity C of the meter. The spectral ?lter i2 is adapted of the fluorescent light in each spectral band with each of a plurality of empirical charts in to pass a predetermined band thereto and the succession respectively, each of said charts cor ?uorescent illumination issuing from the solvent responding to hydrocarbons of different known sample is thus separated into its spectral com ponents. A series of these spectral ?lters such 15 concentrations. 2. The method of exploring for subterranean as the ?lter illustrated are used in succession, a petroleum deposits which consists in, subject separate measurement of intensity being obtained ing a solvent containing the dissolved hydrocar for each ?lter so employed, the measurements be bons and pseudo-hydrocarbons of a measured ing performed in consecutive order until the en tire spectral band has been measured and an 20 quantity of an earth sample to an ultraviolet intensity reading obtained for each portion of radiation of controlled intensity, passing the ?u the band. The standard empirical charts em 'orescent light emanating from the solvent ployed with‘the present invention are prepared by performing this measuring operation with through a sion, each known hydrocarbons of different known concen 25 tively to a intensities trations and plotting the results as a family of plurality of spectral ?lters in succes of said ?lters corresponding respec different spectral band, measuring the of ultraviolet radiation required to intensity curves corresponding respectively to dif produce apredetermined intensity of ?uorescent ferent spectral bands. light in each spectral band respectively, and in ‘comparing the measured ultraviolet intensities . In analysing an earth sample containing an unknown hydrocarbon in accordance with the 30 with each of’ a plurality of empirical charts re spectively corresponding to hydrocarbons of dif method of the present invention, the solution containing the unknown hydrocarbon is placed ferent known concentrations. _ 3. The method of determining the presence of in the vessel 9 and subjected to a predetermined intensity of ultraviolet radiation by adjusting the a petroleum bearing strata in a well being drilled ultraviolet ray absorbing wedge member 1 such for oil which consists in, mixing a. measured 35 that a predetermined one of the calibrations a amount of earth sample from the bore hole with is opposite the point of reference M. The in a predetermined quantity of a non-fluorescent tensity of each of the spectral bands issuing from solvent; subjecting a predetermined fractional the sample is measured by comparing the read portion of said solvent to an ultraviolet radia ings of the meter M with respect to the calibra tion, passing the fluorescent light emanating 40 tion C thereof corresponding respectively to each from the solvent'through a plurality of spectral of the spectral ?lters employed in succession dur ?lters in succession, each of said ?lters corre ing the measuring operation. These measured sponding to a different spectral band respec intensities are now compared with the aforesaid tively, measuring the intensity of the ?uorescent ‘empirical charts and the type and hydrocarbon 45 light in each spectral band, and in comparing ‘content of the sample determined in accordance each of the measured intensities of the fluores with the results of this comparison. What I claim as new and desire to be secured by Letters Patent of the United States is: 1. The method of exploring for subterranean petroleum deposits which consists in, preparing 50 a solution containing a plurality of dissolved hy- -' cent light with a plurality of empirical charts respectively corresponding to hydrocarbons of known concentrations. ' ' ' CHARLES B; BROWN.