ANALYSIS OF CRUDE SHALE OIL - University of Utahrepository.icse.utah.edu/dspace/bitstream/123456789/6842/1/Anal of... · ANALYSIS OF CRUDE SHALE OIL by ... John S., Analytical Distillation

ANALYSIS OF CRUDE SHALE OIL

BY R. F. STEVENS, G. U. DINNEEN, AND JOHN S. BALL

* * * * * * * * * Report o f Investigations 4898

UNITED STATES DEPARTMENT OF THE INTERIOR

Oscar L. Chapman, Secretary

BUREAU OF MINES

J. J. Forbes, Director

Work on manuscript completed January 1952. The Bureau of Mines will welcome reprinting

of this paper, provided the following footnote acknowledgment is made: "Reprinted from

Bureau of Mines Report of Investigations 4898."

The work upon which this report is based was done under a cooperative agreement between

the Bureau of Mines, United States Department of the Interior, and the University of Wyoming,

Laramie, Wyo.

August 1952

ANALYSIS OF CRUDE SHALE OIL

by

R. F. Stevens,-' G. U. Dinneen,—'

and John S. Ball-2'

CONTENTS

Page

Introduction and summary 1

Acknowledgments 1

Apparatus 2

Drying equipment 2

Distillation facilities 2

Equipment for property determinations 2

Procedure 3

Preparation of sample 3

Properties of crude shale oil 3

Distillation of crude shale oil 3

Examination of fractions and residue from distillation ... h

Development of method 5

Distillation 5

Examination of fractions 6

Application of method 9

Conclus ion 20

l/ Formerly chemist, Bureau of Mines, Laramie, Wyo.; present address, University of Wyoming, Laramie, Wyo.

2/ Chemist, Bureau of Mines, Laramie, Wyo. 3/ Chemical engineer, Bureau of Mines, Laramie, Wyo.

Beport of Investigations ^898

TABLES

Page

1. Distribution of sulfur in distillates from crude shale oils. 7

2. Distribution of nitrogen in distillates from crude shale oils 8

3. Comparison of some properties of vacuum fractions from two crude shale oils 9

k. Bureau of Mines crude shale-oil analyses of American and foreign shale oils 10

ILLUSTRATIONS Follows

Fig. page

1. Distillation-analysis equipment, showing pressurized

equipment at right and vacuum equipment at left .... 2

2. Flask for crude shale-oil distillation 2

3. Condenser for crude shale-oil distillation 2

h. Quantity of gas obtained by destructive distillation of 300 ml. of crude shale oil or petroleum 6

^858 - ii -

INTRODUCTION AND SUMMARY

A laboratory method for examining crude shale oil is described. The method uses only about 500 ml. of sample and a limited number of analytical determinations. Results provide information on the general characteristics and composition of an oil and serve as a basis for comparing different oils. However, the method does not provide for direct estimates of yields of commercial products. Analyses of 10 oils produced in the United States by different methods of retorting and of 10 shale oils from commercial-scale operations in 6 foreign countries are given.

The shale-oil-analysis method presented in this paper is based on and employs the same equipment as the Bureau of Mines routine method for analyzing crude petroleum. As shale oil contains groups of compounds not generally found in petroleum, several modifications of the petroleum method that might increase its suitability for application to shale oil were investigated. The modifications included in the present method take into account the apparent poor heat stability of shale oil and the presence of large quantities of olefins and nitrogen compounds.

ACKNOWLEDGMENTS

This project was part of the Synthetic Fuels Program of the Bureau of Mines and was carried out at the Petroleum and Oil Shale Experiment Station, Laramie, Wyo., under the general direction of H. P. Rue and H. M. Thome. The authors wish to thank P. P. Veneziano and G. S. Terrana, who made part of the analyses.

Procurement of the oil samples from foreign countries was arranged by Bureau of Mines personnel during visits to these countries, and acknowledgments are given in the reports^»9>o> 1/ of those visits. The authors appreciate the cooperation of the Union Oil Co. of California and the Tennessee Valley Authority in furnishing samples from operation of their respective retorts.

5/Guthrie, Boyd, and Klosky, Simon, The Oil-Shale Industries of Europe:Bureau of Mines Rept. of Investigations V776, 1951* 73 pp.

5/ Kraemer, A. J., and Thorne, H. M., Oil-Shale Operations in New South Wales, Australia: Bureau of Mines Rept. of Investigations !+796> 1951, ^8 pp.

6/ Thorne, H. M., and Kraemer, A. J., Oil Shale in Spain: Bureau of Mines Rept. of Investigations V736, 1950, 21 pp.

7/ Thome, H. M., and Kraemer, A J., Oil-Shale Operations in the Union of South Africa: Bureau of Mines Rept. of Investigations (in preparation).

!+858 - 1 -

APPARATUS

Drying Equipment

Any equipment, such as a drying oven, flask, tubing, condenser, and receiver,.§/ that provides for the removal of water from the sample without overheating or loss of oil is satisfactory.

Distillation Facilities

The equipment should be suitable for conducting distillations at atmospheric pressure and at a pressure of k-0 mm. of mercury. If the normal atmospheric pressure is less than 700 mm. of mercury, a system pressurized to 760 mm. of mercury9/ should be used.

Figure 1 is a photograph of the equipment at this laboratory. The following special items of equipment are required:

1. A distillation flask, as indicated in figure 2.

2. A wire packing support, formed as shown in figure 2.

3. Approximately 150 gm. of No. 18 jack chain.

h. Four conical wire-gauze spray catchers of such diameter that they will be held in the flask neck by friction.

5. A hemispherical heater capable of maintaining the specified distillation rate.

6. A condenser as shown in figure 3.

7. Magnesia insulation about ^,/k inch thick, shaped to cover the flask from the top of the heater to within about 1 inch of the sidearm.

8. An A.S.T.M. low-distillation thermometer.

9. Test tubes having a capacity of 3° ml. and graduated in 0.2 ml.

10. A fraction collecting device having a capacity of 12 test tubes.

Equipment for Property Determinations

The method presented in this paper employs a number of standard analytical tests. The proper equipment for these tests is required.

87 Guthrie, Boyd, Studies of Certain Properties of Oil Shale and Shale Oil:Bureau of Mines Bull. kl5, 1938, p. 22.

9/ Wenger, Welton J., and Ball, John S., Analytical Distillation of Crude Oils at ~ High Altitudes by the Bureau of Mines Routine Method: Bureau of Mines Rept.

of Investigations 4-517, 19^9, 9 PP.

m% - 2 -

Figure 1. - D is t i l la t ion-ana lys is equipment, showing pressurized equipment at right and vacuum equipment at left .

Figure 2. - Flask for crude shale-oil distil lation.

9±

y&ri\ yyys s yyyyyyys yyyyyy-y-77

ik

'/y/yyy-7~7;

4 *

SOLDER JOINT-

ss s s s sy ; s s y y y y y s s y y j s y y y y y s s s s s s ^ * ^ y y s f .

-SOLDER JOINT

l) 1,1 II

WIRE, & DIA.

- 2 4 THREADS PER INCH

- 32 THREADS PER INCH

S J S J J J S S S J S J S y , » r j s s s ; s s , j s ^ ^

-BRASS TUBING, it THICK

6 * -

I s s y y s s s y y y y y s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s y s y y s s y ; ;

LEAD WASHERS

; - £ ALL DIMENSIONS IN INCHES

Figure 3. - Condenser for crude shale-oil distil lation.

PROCEDURE

Preparation of Sample

Many crude shale oils contain a substantial quantity of water. This water is often present in the form of a stable emulsion so that distillation is the most convenient method for its removal. A representative sample of about 500 ml. should be dried until no appreciable amount of water remains in it. The water content should be recorded so that it may be reported when it is of interest.

Properties of Crude Shale Oil

The gravity,i2/ sulfur content,±±J nitrogen content,±tJ pour point, 13/ and viscosity at 100° F .1̂ 7 are obtained on the dried sample.

Distillation of Crude Shale Oil t

A 300-ml. sample of the dried oil is distilled into 1^ fractions, each having a nominal boiling range of 25° C. The first seven are obtained at a pressure of about 760 mm. of mercury, and the remainder are distilled at a pressure of h-0 mm. of mercury.

The tare weight of a distillation flask and boiling chips is obtained. The weight of oil equivalent to a volume of 300 ml. is calculated from the specific gravity. This amount is weighed into the flask containing half the tared boiling chips, care being taken not to get any oil into the side arm of the flask. The device for supporting the jack chain in the neck of the flask is adjusted so the lower spiral is about on a level with the point at which the flask neck starts to widen into the bulb. The jack-chain packing is placed in position so it fills the flask neck to within about 1 inch of the sidearm. It can be packed to fill the required space as it is put in by tapping the flask neck with the fingers. The thermometer is inserted in the flask so that the top of the bulb is about l/l6 inch below the bottom of the sidearm when the cork is pressed firmly into the flask neck. The flask, heater, condenser, receiver, and test tubes are assembled on the distillation rack. Ice is placed in the condenser and receiver; and, if necessary, the system is pressurized to 76O mm. of mercury.

When the apparatus is completely assembled, input to the heater is adjusted so distillation begins in about 15 to 20 minutes. The thermometer reading is recorded

107 See footnote 8, p. 26. ll/ American Society for Testing Materials, Standard Method of Test for Sulfur in

Petroleum Products and Lubricants by the Bomb Method (D129-1+9): 19^9 Book of A.S.T.M. Standards, part 5, Philadelphia, 19*4-9, pp. 770-772.

12/ Lake, G. R., McCutchan, P., Van Meter, R., and Neel, J. C, Effects of Digestion Temperature on Kjeldahl Analyses: Anal. Chem., vol. 23, Nov. 1951> pp. 163^-1638.

13/ American Society for Testing Materials, Standard Method of Test for Cloud and Pour Points (D97-1+7): 19*4-9 Book of A.S.T.M. Standards, part 5, Philadelphia,

19^9, PP. 736-739. lk/ American Society for Testing Materials, Standard Method of Test for Viscosity

by Means of the Saybolt Viscosimeter (D88-M4-): 19^9 Book of A.S.T.M. Standards, part 5, Philadelphia, 19^9, pp. 701-705-

W58 - 3 -

when the first drop falls from the end of the condenser, and the heater is regulated so that condensate is collected at a rate of h to 5 ml. per minute. The first fraction is cut at 50° C., and a fraction is taken for each subsequent temperature interval of 25° C. When a thermometer reading of 200° C. is reached, the heater is turned off and lowered from the flask immediately to prevent further distillation. After the condenser has drained, the tubes containing the fractions are removed from the receiver, closed with corks having the appropriate fraction numbers, and placed in a 60° F. bath.

When the flask is cool, the thermometer, jack-chain packing, and packing support are removed. The remaining tared boiling chips are placed in the flask, and the four conical wire-gauze spray catchers adjusted in the neck of the flask at intervals between the bulb and the sidearm. The thermometer is replaced and the apparatus assembled for the distillation at a pressure of k-0 mm. of mercury. To maintain a satisfactory vacuum, it may be necessary to lute the corks with a paste of litharge and glycerin. The magnesia insulation is used during the vacuum distillation, and an immersion heater is employed to raise the temperature of the condenser water from about 50° to 80° C. during the distillation.

When the pressure of the system has been regulated at kO mm. of mercury, the heater is turned on and adjusted so that distillation starts in a reasonable time. The distillation rate is the same, k to 5 nil. per minute, as in the distillation at atmospheric pressure, and it is essential to maintain this rate if reproducible results are to be obtained. The first vacuum fraction, which is number 8 on the basis of the total oil, contains all the material distilling below 150° C. The remaining fractions are taken at 25° C. intervals to 300° C. When this latter temperature is reached, the current is turned off and the heater lowered from the flask. If extensive cracking occurs before a temperature of 3OO0 C. is attained, the distillation is stopped and the maximum temperature recorded. The tubes containing the fractions are removed from the receiver, closed with corks having the appropriate numbers, and placed in the 60° F. bath. The flask containing the residuum is cooled, weighed, and the residuum saved for property determinations.

Examination of Fractions and Residue from Distillation

Some of the analytical determinations are made on the individual fractions as obtained in the distillation, whereas others are made on selected volumetric composites.

The volumes of the fractions are obtained at 60° F. if they are fluid at that temperature. Fractions that are solid at 60° F. are heated to 100° F., the volume determined, and the result converted to volume at 60° F .i^/ The specific gravity is obtained on each of the fractions. Depending on the volume of the fraction, the determination is made, using either a specific-gravity balance or a pipette pycnom-eter.lo/ Aniline point is determined on each of the fractions obtained in the vacuum distillation.17/ As the volume of the fraction may be small, 5 nil. each of sample and of aniline is ordinarily used. The kinematic viscosity is obtained on each of

15/ Bureau of Standards, National Standard Petroleum Oil Tables: Circ. C4l0, 1936, 172 pp.

16/ Smith, N. A. C, Smith, H. M., Blade, 0. C, and Garton, E. L., The Bureau of Mines Routine Method for the Analysis of Crude Petroleum, I, The Analytical Method: Bureau of Mines Bull. ̂ 90, 1951, PP- 32-3^.

17/ American Society for Testing Materials, Tentative Method of Test for Aniline Points and Mixed Aniline Points of Petroleum Products (D611-47T): 19^9 Book of A.S.T.M. Standards, part 5, Philadelphia, 19^9, pp. 9^9-95^.

U858 - k -

the fractions from 11 to lk.]&/ This kinematic viscosity is converted to Saybolt Universal seconds.19/

After tests on the individual fractions have been completed, the following composites by volume are prepared: Naphtha from the fractions up through number 7> light distillate from fractions 8 to 10, and heavy distillate from fractions 11 to Ik. The nitrogen content of each of these composites is determined.20/ On the naphtha and light distillate, the tar-acid21/ and tar-base21/ contents are determined, and hydrocarbon-group analyses

2l/22j are run on the neutral oils after removal

of tar acids and tar bases. The specific gravity of the residuum is obtained by a pycnometer method ,12/

which may be modified as follows: (l) The pycnometer may be either straight-walled or pear-shaped, with a stopper diameter of approximately 22 mm., and (2) the determination is made at 15.6° C. instead of at 25° C. Nitrogen content and carbon res are obtained on the residuum. As residua from shale oil have a decided tendency to froth in the carbon residue determination, it is often necessary to reduce the sample size so deviations from the recommended time schedule are permitted and only approximate results are obtained.

DEVELOPMENT OF METHOD

Shale oil is a source of liquid fuels similar to those obtained from petroleum. Unfortunately, the two materials are sufficiently different so' that the same analytical method cannot be used satisfactorily for both. Consequently, the procedure2!?/ employed by the Bureau of Mines for many years for analyzing crude petroleum was used as a basis and modified to make it applicable to crude shale oil.

Distillation

When crude shale oil is distilled, visual observation sometimes indicates the occurrence of thermal decomposition before a vapor temperature of 275° C. (the cut point of the atmospheric distillation in the crude-petroleum method) is reached.

18/American Society for Testing Materials, Tentative Method of Test for Kinematic-

Viscosity (DM^-^T) Method B: 19^9 Book of A.S.T.M. Standards, part 5, Philadelphia, 19^9, pp. 906-909.

19/ American Society for Testing Materials, Standard Method for Conversion of Kinematic Viscosity to Saybolt Universal Viscosity (DM+6-39) : 19I+9 Book of A.S.T.M. Standards, part 5, Philadelphia, 19^9, pp. 910-911.

20/ See footnote 12. 21/ Dinneen, G. U., Bailey, C. W., Smith, J. R , and Ball, John S., Shale Oil

Naphthas, Analysis of Small Samples by the Silica-Gel Adsorption Method: Anal. Chem., vol. 19, December I9V7, pp. 992-999.

22/ Dinneen, G. U., Thompson, C. J., Smith, J. R., and Ball, John S., Adsorption Analysis by Displacement Techniques as Applied to Shale-Oil Distillates: Anal. Chem., vol. 22, July 1950, pp. 87I-875.

23/ American Society for Testing Materials, Standard Method of Test for Specific Gravity of Road Oils, Road Tars, Asphalt Cements, and Soft Tar Pitches (D70-27): I9I+9 Book of A.S.T.M. Standards, part 3, Philadelphia, 19^9, pp. 1098-1099.

2k/ American Society for Testing Materials, Standard Method of Test for Carbon Residue of Petroleum Products, Conradson Carbon Residue (Dl89-1+6) : 19^9 Book of A.S.T.M. Standards, part 5, Philadelphia, 19^9, pp. 801-80^.

25/ See footnote 16.

I+858 - 5 -

Although the decomposition may not be serious, it is preferable to stop atmospheric distillation of crude shale oil at a lower temperature than this. A value of 200° C. was selected because it is well below decomposition temperatures and also the total atmospheric distillate obtained'approximates a 200° C. end-point naphtha. The vacuum distillation is continued to a vapor temperature of 300° C. (as in the petroleum method), unless extensive decomposition is noted earlier.

To obtain information on the relative heat stability of shale oil and petroleum, atmospheric distillations of several samples of each were continued until large volumes of noneondensable gas were liberated. The equipment was similar to that used , in the method, except that provision was made for obtaining liquid temperatures and for measuring and collecting the gas produced. Figure k shows a plot of gas collected vs. liquid temperature for a shale oil produced by the gas-combustion process and for a low-sulfur crude petroleum. The results for the gas-combustion oil are similar to those obtained on another shale oil and a Wyoming black oil. In plotting the data in figure k, gas collected before distillate was obtained was ignored, as it was assumed that this gas resulted from displacement by condensable vapors. If gas production is used as a criterion, it is apparent that the shale oil decomposes under the conditions of this experiment at about k0° C. lower than does the petroleum. However, only small quantities of gas are produced below a liquid temperature of 375° C., which corresponds in these runs to vapor temperatures of 305° to 310° C. As the analytical procedure employs somewhat lower temperatures than these, it appears that thermal decomposition will seldom cause serious errors.

The cut temperature of 200° C. for atmospheric distillation of shale oil is 75° C. lower than in the method for petroleum. A corresponding decrease in the cut temperature for the first fraction of the vacuum distillation would indicate that, for shale oil, this fraction should be taken up to 125° C. However, because the decreased pressure causes less reduction in vapor temperature at 200° C. than at 275° C., it has been found that the initial boiling point in the vacuum distillation is only slightly below 125° C., so the first vacuum fraction is taken up to 150° C. Thus a total of lk fractions is obtained from the distillation.

Examination of Fractions

Analysis of the fractions from the distillation should yield a reasonable amount of information concerning the composition of the oil. It is particularly necessary to take into account the large amounts of unsaturated hydrocarbons and the sulfur, nitrogen, and oxygen compounds that are present. However, the work should not be unduly extensive.

Determination of hydrocarbon groups by adsorption is the most reliable^/ method now available for analyzing complex materials, such as shale oil. This determination, as well as extraction of tar acids and tar bases, a necessary preliminary step, is made on volumetric composites prepared from fractions 1 to 7 (naphtha) and fractions 8 to 10 (light distillate). Composites rather than individual fractions are used because these analyses require rather large samples. Even composite samples are seldom large enough to give accurate results for tar acids and tar bases, but the determinations are included in the method to give some information on these types of material. Unfortunately, these methods are not applicable to higher-boiling distillates, so for fractions 11 to ik aniline point and viscosity are used for

267 Dinneen, G. U., Smith, J. E., and Ball, John S., Olefins in Naphtha: Petrol. Refiner, vol. 29, No. 3, May 1950, pp. 129-13^.

4858 - 6 -

7000

z o

o z o o

6P00 -

5P00 -

o SHALE OIL

a PETROLEUM

l -

r 4,000

UJ

| 3,000 >

<

UJ >

- I

2P00

ipoo —

_ Q i -CUta k-o. 200 250 3 0 0 3 5 0 4 0 0

LIQUID TEMPERATURE, °C.

4 5 0

Figure 4. - Quantity of gas obtained by destructive distillation of 300 ml. of crude shale oil or petroleum.

characterization even though they are not particularly satisfactory. To provide a better correlation between these properties and the hydrocarbon group analyses, aniline points are also determined on fractions 8 to 10.

Specific gravity and carbon residue are the only determinations normally made on the residuum. In certain instances where significant quantities of ash may be present in the shale oil, an ash determination is made after the carbon-residue determination.

As shale oils always contain substantial quantities of sulfur and nitrogen, distribution of these elements with respect to boiling range might be significant in characterization studies. To investigate this possibility, sulfur and nitrogen were determined on each of the composites and on the residuum from a number of shale oils for which complete analyses are given later in this paper. The results are shown in tables 1 and 2. The sulfur contents of the fractions from any given oil are all of about the same magnitude. For the oils from Colorado shale, the sulfur content tends to be lower in the higher-boiling fractions. For the rest of the oils, an opposite tendency is apparent. However, the trends are not pronounced, so determination of sulfur on the fractions provides little information in addition to that obtained from a sulfur determination on the crude shale oil.

The results in table 2 show that the nitrogen content of the fractions increases greatly with boiling range. Therefore, a nitrogen determination on each of the fractions in the distillation summary is included in the analytical method.

TABLE 1. - Distribution of sulfur in distillates from crude shale oils

Country and retort U. S. A., N-T-U U. S. A., gas combustion U. S. A., Pumpherston U. S. A., gas flow U. S. A., Royster U. S. A., Parry U. S. A., 1,200° F. high-temp. U. S A., 1,500° F. high-temp. U. S. A., Royster - T. V. A. . Spain, Pumpherston-type South Africa, Salermo Australia, Pumpherston Sweden, Rockesholm Sweden, Ljungstrom Scotland, Pumpherston France, Pumpherston France, Marscaux France, Cantieny France, Lantz

Sulfur content of fraction, weight percent

Naphtha Light

distillate "033~ .81 .80 .69 .71 .98 .78 .76

2.30 .30 .60 .53

1.33 .75 .30 .39

2.79 2.85

.<?k

Heavy distillate Residuum

0.77 1.03 .8^ •71 .81 .89 .79 .75

2.3^ .27 M .ki

l.lj-2

• 70 .27 .k2

3.17 2.9^

0.79 .70 .56 .65 .67 .89 .81

.7^ 2.98 .36 .60 .5k

l.kf

.29

.ko ,82 .26 .62

0.70 .65 .61 .58 .60 .87 .79 .7^

3.35 .ko .55 .57

1.69

M .53

2.85 3.2k • 69

^858 - 7 -

TABLE 2. - Distribution of nitrogen in distillates from crude shale oils

Country and retort

Nitrogen

Naphtha

content of fraction, weight percent Light

distillate Heavy

distillate Residuum

u. u. u. u. u. u. u. u. u.

s. s. s. s. s. s. s. s. s.

A A A A A A A A A

N-T-U gas combustion Pumpherston gas flow Royster Parry 1,200° F. high temp. 1,500° F. high temp. Royster - T. V. A.

Spain, Pumpherston-type South Africa, Salenno Australia, Pumpherston Sweden, Rockesholm Sweden, Ljungstrom Scotland, Pumpherston France, Pumpherston France, Marecaux France, Cantieny France, Lantz

.17

.17 51 ,30 .99 .51 97 30 ,22 ,18 ,11+ ,10

• 17 07 13 1+0

15 .16 11

.37

.18 ,21

.27

2.37 3.20

• 31 .38 .50 .21+ .30 .13 M .58

• 35 .37 • 27

.60

.03

.91+

.79

.79 • 70 .26 .11 .75 .76 .85 .50 .62

.82

.85

.65

.81

2.01+ 2.1+7 3.00

.1+8

.28

.50

.71

.02

.1+1+

.15

.30

.81

.97

1.28 I . 3 6 1.01+ 1.11+ 1.20

As mentioned previously, this shale-oil analysis procedure is based on the Bureau of Mines routine method for crude petroleum. Two values - cloud point and correlation index27/ - which are reported in the petroleum method are omitted from the shale-oil procedure. Cloud points were determined on fractions from crude shale oils obtained from a number of sources. Differences among the values obtained were too small to make the cloud point useful as a characterizing factor.

Although correlation index and other boiling point-gravity factors28/29/ are widely used in the petroleum industry as indexes to composition, no such factor is reported in this method for analyzing shale oil. These constants, particularly characterization factor, have been correlated empirically with a great many properties of petroleum fractions. The presence in shale oil of large quantities of non-hydrocarbons and of hydrocarbons differing from those in petroleum make it difficult to predict to what extent these correlations are valid for shale oil. In general it seems that, for shale oil, the most-reliable correlations would be those that predict physical properties such as molecular weight, while the least reliable would be those that predict properties dependent largely on chemical structure, such as aniline point, viscosity, or octane number. The latter difficulty is illustrated by the oils shown in table 3> which have fractions with similar boiling point-gravity constants but different chemical compositions. As the distillation is standardized, differences in the boiling point-gravity factors for the two oils come essentially

27/ Smith, H. M., Correlation Index to Aid in Interpreting Crude-Oil Analyses: Bureau of Mines Tech. Paper 610, I9I+0, 3I+ pp.

28/ Jackson, E. A., Boiling Point-Gravity Constant Is Index of Lube-Oil Character-istics: Oil and Gas Jour., vol. 33, Mar. 21, 1935, p. l6.

29/ Watson, K. M., and Nelson, G. F., Improved Methods for Approximating Critical and Thermal Properties of Petroleum Fractions: Ind. Eng. Chem., vol. 25,

August 1933, PP. 88O-887.

1+858

from the gravity term. The similarity in gravity but difference in aniline point and viscosity, indicating the greater aromaticity of the Eockesholm oil, is evident. In certain instances application of these factors to shale oil should yield valuable data and may be necessary for processing calculations. However, it did not appear advisable to include such a factor as a standard part of the method.

TABLE 3. - Comparison of some properties of vacuum fractions from two crude shale oils

Fraction No. 8 9 10 11 12 13 Ik

Oil from Sweden, Eockesholm retort Specific gravity, 60°/60° F. 0.89^ .926 .955 .976 .99^

1.001+ 1.033

Aniline point,

°C. Below 0 Below 0 Below 0 Below 0 Below 0 Below 0 Below 0

Viscosity at 100O F., centistokes

10.0 22.7 65.8

352. k

Oil from France, Cantieny retort Specific gravity,

60°/60° F. O.898 .917 .9̂ 1 .962 .993

1.012 l.OllO

Aniline point,

°C. Ik.k 17.0 20.0 21.9 18.2 28.8 30.8

Viscosity at 100° F., centistokes

7 A 15 A 35.9 107.2

APPLICATION OF METHOD

Eesults obtained on 20 crude shale oils by the method described in this paper are presented in table k. The oils are designated by the country in which they originated and the retort in which they were produced. The oils are from 7 countries, as follows: 10 from the United States of America, 1 from Spain, 1 from the Union of South Africa, 1 from Australia, 2 from Sweden, 1 from Scotland, and k from France. Eight of the American oils were produced from Colorado shale by various experimental operations of the Bureau of Mines, one was produced by the Union Oil Co. and is also from Colorado shale, and the remaining one was produced from Tennessee shale by the Tennessee Valley Authority. The samples from foreign countries were from commercial-scale processing in those countries.

Many different retorts were used to produce the oils, but they usually fall into one of three general classifications that have been proposed: 39_/ (1) Those in which heat is transferred to,the shale through a wall, as represented by the Pumpherston, Parry, Eockesholm, Marecaux, Cantieny, and Salermo retorts; (2) those in which heat is transferred to the shale from combustion gases generated in the retort, as represented by the N-T-U, gas combustion, and Union Oil Co. retorts; and (3) those in which heat is transferred to the shale by passing previously heated gases through the shale bed, as represented by the gas-flow, Eoyster, and Lantz retorts. In addition, oils from two unusual processes are included. The essential feature of the high-temperature process is rapid conversion of organic matter to oil at temperatures substantially above those employed by usual retorting procedures. Analyses of oils produced by operation of this process at two temperatures, 1,200° and 1,500° F., are given. The Ljungstrom process is unique in that it uses tubular electric heaters to heat the oil shale in place and thus recovers only volatile products.

30/ Cattell, E. A , Guthrie, Boyd, and Schramm, L. W., Eetorting Colorado Oil Shale - a Beview of the Work of the Bureau of Mines, U. S. Department of the Interior: 2d Oil-Shale and Cannel-Coal Conference, Glasgow, 1950.

31/ The retort used in Spain has tubes of elliptical cross section similar to those of the Henderson retort. The oil produced is classed in this paper as Pumpherston-type, since the Spanish retort, like the Pumpherston, is a vertical, externally heated retort.

>l858 - 9 -

TABLE 4. BUREAU OF MINES CRUDE SHALE-OIL ANALYSES OF AMERICAN AND FOREIGN SHALE OILS

Source of shale: Rifle, Colorado, U. S. A. Eduction method: N-T-U (Nevada - Texas - Utah) retort Source of shale:

Eduction method: Rifle, Colorado, U. S. A. Gas Combustion retort

PROPERTIES OF CRUDE SHALE OIL

Specific gravity A.P.I, gravity Sulfur, percent Nitrogen, percent Pour point, °F. Viscosity, S. U. seconds at 100°F.

0.935 19.8

.71, 1.78 90

280

Naphtha (Frac. 1-7) Light distillate

(Frac. 8-10) Heavy distillate

(Frac. 11-11.) Residuum Loss

Volume percent 2.7

15.7

3U.U 1.5.8 1.1s

PROPERTIES OF COMPOSITE FRACTIONS

Sp. (jr. "A.P.I. 0.791 1.7.1.

.872 30.8

.913 23.5

.980 12.9

Nitrogen, percent

1.17

1.21.

1.60 2.0b


Specific gravity A.P.I, gravity Sulfur, percent Nitrogen, percent Pour point, °F. Viscosity, S.U.

0.91.3 18.6 .69

2.13 85

Naphtha (Frac. 1-Light distillate

(Frac.8-10) Heavy distillate

(Frac.11-110 Residuum

•7)

Volume. percent

1..1.

11*.6

31.3 1.9.7


Sp. gr. 'A.P.I. 0.822 1.0.6

.872 30.8

.927 21.1

.986 12.0

Nitrogen, percent

1.17

1.37

2.03 2.1.7

seconds at 100"F. 310 Loss

DISTILLATION AND ANALYTICAL DATA

Distillation at 760 mm. Hg Sum,

Frac. Cut at- Per- per- Spec. No. *C. °F. cent cent grav.

Analysis of Naphthai/

50 122" 75 167 100 212 125 257 150 302 175 31.7 200 392 2.7 2.7 0.791

Tar Acids Tar bases Neutral oil:

Paraffins and naphthenes

Olefins Aromatic s*

3.0 7.8

33 1.8 19

Light dist. (Frac.1-7), (Frac.8-10), in percent in percent

37 31. 29

..Includes some sulfur and nitrogen compounds.

Frac. No.

8

Cut at-•C. °F. 150 302

Percent 3.1.

Distillation at 1.0 mm. Hg Sum, Gravity per- Specific, 'A.P.I., cent 60°/60° F. 60° F. 6.1 0.051. 31..2

Aniline point, °C. 37.1.

Vis. at 100°F. K.V., S.U., c.s. sec.

9 10

11 12 13 11.

Residuum

175 317 200 392

5.3 11.1. 7.0 18.li

225 250 275 300

1.37 1,82 527 572

8.3 7.2 7.9

11.0

1,5.8

26.7 33.9 1,1.8 52.8

98.6

.861,

.886

.891,

.905

.920

.929

.980

32.3 28.2

26.8 21,. 9 22.3 20.8

12.9

37.8 U.6

1.3.8 1.5.0 50.6 56.8

10.6 13.6 22.7 1,0.8

59 72

110 190

Carbon residue of residuum, 7-5 percent; carbon residue of crude, 3.6 percent,

1/ These results obtained on sample from larger-scale distillation.

1+858


Distillation

Frac. No.

Cut °C.

at-

7F

at 760

Percent

mm. Sum, percent

Hg

Spec. grav.

Analysis of—

50 122 75 167 100 212 125 257 150 302 175 31.7 200 392

1.5 2.9

1.5 0.806 U-U .831

Tar acids Tar bases Neutral oil:


Olefins Aromatics»

Naphtha Light dist. (Frac.1-7), (Frac.8-10), in percent in percent

7T 7.5

27 51 22

5TT 10.5

27 1.2 31

..Includes some su l fu r and ni t rogen compounds.

D i s t i l l a t i o n at 1,0

Frac . No.

Cut a t -~°F7

9 10

11 12 13 11.

Residuum

~T50~l02 175 31.7 200 392

Percent

Sum, pe r cent

Gravity _Hg_

3 7 2 7 7 6 " " 5.7 13.3 5.7 19.0

Specif ic , 60/60° F.

225 1.37 5.9 2L.9 250 1,82 7.6 32.5 275 527 7.6 1,0.1 300 572 10.2 50.3

1,9.7 100.0

0.81,9 .867

.899

.915

.935

.91,5

.986

'A .P . I . , 60° F. isrr

31.7 27.7

25.9 23.1 19.8

18.2

12.0

Aniline point, •c.

Vis, at 100° F. K.V.

32.1. 33.5 31.1.

31,. 8 33.6 32.9 38.3

S. U. sec.

8.2 15.2 32.1 68.1,

53 78

150

315

Carbon residue of residuum, 5.2 percent; carbon residue of crude, 2.7 percent.

10 -

TABLE 4. (Cont.)

Source of shale: Eduction method:

Rifle, Colorado, U. S. A. Pumpherston retort

Source of shale: Rifle, Colorado, U. Eduction method: Gas Flow retort

S. A.



seconds at 100°F.

0.900 Naphtha (Frac.1-7) 25.7 Light distillate

.77 (Frac.8-10) 1.57 Heavy distillate

60 (Frac.11-1^) Residuum

50 Loss


Volume, percent -§E^g£ "A.P.I .

17.6 0.805

29.14

ho.o 12.7

.3

.873

.927

.010

hli.3

30.6

21.1 8.6

Nitrogen, percent

o.Si

1.18

1.9L 3.00


Speci f ic g rav i ty A . P . I , g rav i ty Su l fur , percent Nitrogen, percent Pour p o i n t , "F. Viscos i ty , S.U.

seconds at 100°F.

0.959 16.0

.51 2.10

70

660

Naphtha (Frac.1-7) Light d i s t i l l a t e

(Frac.8-10) Heavy d i s t i l l a t e

(Frac .11- lh) Residuum Loss

Volume, percent

1.5"

12.8

25.3 60.0

.1.


Sp. g r . ' A . P . I . 0.8U6 35.8

.880 29.3

.926 21.3

.995 10.7

N i t rogen , p e r c e n t

1.30

1.21

1.79 2.I18


D i s t i l l a t i o n at 76C

Frac. Cut a t - Per-No. °C. *F. cent

1 mm. Hg Sum, p e r - Spec. cent grav.

Analysis of —

9 10

11 12 13 Hi

-50

75 100 12s ISO 175

122 167 212 257 302 317

0.6 3.7 6.0

O.768

.803 200 392 7.3 17.6 .829

0.6

h.3 10.3


Paraffins and

naphthenes Olefins Aromatics*

Naphtha Light dist. (Frac.1-7), (Frac. 3-10), in percent in percent

32 1.3 25

27T 11.5

28 35 37

Încludes some sulfur and nitrogen compounds

Distillation at 1.0 mm. Hp;

Frac.

No.

Cut at-

'*c~. °F7

Percent

Sura, percent

Gravity

150 302 7TB 2FTTT 175 31)7 9.8 35.2 200 392 11.8 1.7.0

Specif ic , 6 0 7 6 0 ° F .

2 25 250 275 300

137 1182 527 572

10.3 10.7 10.1 8.9

57.3 68.0 78.1 87.0

Residuum 12.7 99.7

0.852 .870 .890

.901

.918

.91.2

.9U9

1.010

"A.! 60'

Aniline poin t ,

"C.

Vis . a t 100" F.

3U75~ 31.1 27.5

25.6 22.6 18.7 17.6

8.6

. 5 .

3176 33.2 36.2

1/

I 7.6

11.2 25.9 S3.).

S.U., s e c .

51 71.

125 250


D i s t i l l a t i o n at 760 mm. Hg

Frac . No.

Cut a t -*C. "F.

Percent

Sum, p e r cent

Spec. grav.

Analysis of-

1 2 3 li 5 6 7

So 75

100 125 150 175 200

122 167 212 257 302 31.7 392

Frac. No.

9 10

11 12 13 111

1.5 1.5 0.81.6

Tar acids Tar bases Neutral o i l :


Olefins Aromatics*

2.6 8.2

27 1.2 31

Naphthal/ Light "dist. Frac. 1-7), (Frac.8-10), in percent in percent

T7T 11.5

27 1»3 30

Încludes some su l fu r and n i t rogen compounds.

Cut a t --Tf-

T 5 o ~ 302 175 31.7 200 392

Pe r cent

Sum, pe r cent

D i s t i l l a t i o n at 1.0 mm. Hg Gravity

2.7 1».1» 5.7

225 250 275 300

1.37 1.82 527 572

T 7 T 8.6

1L.3

20.8 26.9 33. li 39.6

Specif ic , 60°/60° F.

Residuum 60.0 99.6

0.871 .877

.903

.921

.936

.91.6

.995

•A.P.I . , 60° F.

Ani l ine p o i n t ,

•C.

V i s . a t 100° F . K.V., c . s .

31.0 29.9 28.2

25, 22, 19. 18.

30.1. 31.8 33.8

36 .h 1.0.1. 1.3.3 1.7.8

7.7 13.3 25.3 53.3

S.U. s e c .

S i 70

119 21.5

10.7

Carbon residue of residuum, 12.0 pe rcen t ; carbon residue of crude, 1.7 percent .

1/ Not determined.

1*858

Carbon residue of residuum, 11.5 pe rcen t ; carbon res idue of crude, 7.2 pe rcen t ,

1/ These r e s u l t s obtained on sample from l a r g e r - s c a l e d i s t i l l a t i o n .

Source of shale: Rifle, Colorado, U. S. A. Eduction method: Royster retort


Specif ic g r a v i t y A .P . I , g rav i ty Sulfur , pe rcen t Nitrogen, percent Pour p o i n t , °F. Viscos i ty , S.U.

seconds at 100 *F.

0.936 19.7

.67 1.97

90

230



(Frac . 11-11,) Residuum Loss

Volume, percent

U.9

13.2

31.6 5o.2

.1

PROPERTIES OF COMPOSITE

Sp. g r . 0.H21

.869

.912

.977

FRACTIONS

•A.P . I . 1.0.9

31.3

23.7 13.3

Nitrogen, percent

0.99

1.27

1.79 2.28


D i s t i l l a t i o n

Frac . No.

Cut *C.

a t -*F.

a t 760

Per cent

mm. Hg Sun, p e r cent

Spec, grav.

Analysis of-Naphthal/

.1-77,

To 75

100 125 150 175 200

122 167 212 257 302 31,7 392

0.2 .3

1.2 3.2

2 ) 5 )0.806 7 ) 9 .629

Tar acids Tar bases Neutral oil: Paraffins and naphthenes

Olefins Aromatics-*

Light dist. (Frac.l-7T, (Frac.8-10), in percent in percent

T7 17.0

27 11 32

Încludes some sulfur and nitrogen compounds.

Distillation at 1.00 Hg

Frac. No.

Cut at-•C. *F. ISO 302 175 31.7 200 392

Percent

Sum, percent

Gravity Specific, 60760° F. "OFT

.868

.880

.889 • 90li .917 .927

.977

•A.P.I. 60° F.

Aniline point,,

Vis. at 100° F. K.V. S.U.,

sec.

9 10

11 12 13 lii

225 250 275 300

1.37 1.82 527 572

3.B U.6 U.8

b.U 6.8 7.1.

11.0

877 13.3 18.1

21. 31. 38. J.9.

Residuum 50.2 99.9

3U.0 31.5 29.3

27.7 25.0 22.8 21.1

13.3

30.1 31..0 36.6

1.7.8 18.8 57.8 65.5

7.0 11.5 19.2 37.8

1.8 61, 91.

175

Carbon residue of residuum, 7.2 percent; carbon residue of crude. 3.8 percent.

1/ Insufficient sample for analysis.

1*858

4. (Cont.)

Source of sha le : Eduction method:

R i f l e , Colorado, U.S.A. Parry r e t o r t


Specif ic g rav i ty A . P . I , g rav i ty Sulfur , percent Nitrogen, percent Pour p o i n t , °F. Viscos i ty , S.U.

seconds at 100"

0.931 20.5

.72 1.73

70

F. 155

Naphtha (F rac . 1-7) Light d i s t i l l a t e

(Frac . 8-10) Heavy d i s t i l l a t e

(Frac . 11-11.) Residuum Los 8

Volume, percen t

8 .0

20.3

33 .6 35 .0

3 . 1

PROPER! COMPOSITE

Sp. g r . 0.812

.863

.928 1.009

riES OF FRACTIONS

• A . P . I . 1.2.8

32 .5

21 .0 8.7

N i t rogen , p e r c e n t

0 .51

.98

1.70 2.50


D i s t i l l a t i o n at 760 mm. Hg Sum,

No. 1 2 3 1» 5 6 7

•c. 50 75

100 125 150 175 200

• F . 122 167 212 257 302 3U7 392

cent

0.5 2.5 5.0

cent

0.5 3.0 8.0

grav.

0.785 .791. .823

Analysis of — Naphtha

(F rac . 1 -7) , in percen t

L igh t d i s t . ( F r a c . 8 - 1 0 ) ,

i n pe rcen t Tar ac ids Tar bases Neutral o i l :

Paraf f ins and naphthenes

Olefins Aromatics*

1 1»

27 1.8 25

U.6 9.7

26 US 29

Încludes some s u l f u r and n i t r o g e n compounds.

Frac . No.

Cut a t -•C. °F.

Percent

D i s t i l l a t i o n at 1.0 mm. Hg Sum, Gravity p e r - Spec i f i c , ' A . P . I . , cent 60°/60° F. 60» F.

Anil ine po in t ,

°C.

V i s . a t 100° F . K.V., S.D., c . s . s e c .

9 10

11 12 13 111

Residuum

150 302 175 31.7 200 392

225 250 275 300

1*37 1.82 527 572

T . 3 13.3 8.0 21.3 7.0 28.3

7.3 7.3 8.0

11.0

35.6 1.2.9 50.9 61.9

35.0 96.9

O.8U1 .861. .877

.900

.911.

.935

.950

1.009

36\2 32 .3 29.9

25.7 23.3 19.8 17.5

8.7

isnr 25.8 30.2

ia.6 1.8.0 55.0 55.2

2 .8 7.1.

51 .6 58.9

35 50

21.0 272

Carbon res idue of residuum 19.5 pe rcen t ; carbon res idue of crude, 7.1. percent

12 -


Rifle, Colorado, U.S.A. High temperature retorting at 1200° F.



seconds at 100°

0.956 16.5

.8U 2.16

60

F. U7

Naphtha (Frac . 1-7) Light d i s t i l l a t e


(Frac . l l - l l i ) Residuum Loss

Volume, percent

39.2

13.5

19.7 27.2

.14

PROPERTIES OF COMPOSITE FRACTIOUS

sP-„6r-0.813

.937

1.129

" A . P . I .

19 . s

11.7

Nitrogen, percent

0.97

2.37

3.26 3.71


Distillation at 760 mm. Hg Analysis of-

•ac. lo. 1 ? 3 U 5 6 7

Cut °C. •in 75

100 125 150 175 200

a t -°F. 1?2 167 212 257 302 31.7 392

Percent 1.2 7.2 5.7 7.0 5.9 5.7 6.5

Sum, pe r cent 1.2 8.a

l l i . l 21.1 27.0 32.7 39.2

Spec. grav. 0.705

.7u3

.795

.816

.830 •8U7 .877

Frac. No.

9 10

11 12 13 111


Paraff ins and naphthenes

Olefins Aromatics*

1.2 9.2

10 39 51

Naphtha Light dist. (Frac. 1-7), (Frac.8-10), in percent in percent nrr

(1 / )

10 29 61

Încludes some sulfur and nitrogen compounds

Distillation at liO mm. Hg

Cut a t -°F.

Percent

150 302 175 3U7 200 392

225 U37 250 1.82 275 527 300 572

T3" 6.2 I1.8

Sum, pe r cent

Gravity

TUTT Ii7.9 52.7

Specif ic , 60760° F.

Residuum

U.O 56.7 3.9 60.6 U.l 61..7 7.7 72.li

27.2 99.6

0.911i .932 .951.

.97li

.981

.995 1.008

1.129

"A.P.I . , 60° F.

Anil ine poin t ,

°C.

Vis . a t 100" F.

23.3 20.3 16.8

13.8 12.7 10.7 8.9

below 25 below 25 below 25

below 25 28.2 36.8 li3.U

K.V., c . s .

S.U., s e c .

8.1. 18 .1 31.3 70.2

53 90

1I18 330

rarhnn residue of residuum. 31..U percent ; carbon res idue of crude, 11.1 percent,

l/ Not determined.

1.858

4. (Cont.)

Source of shale: Rifle, Colorado, U.S.A. Eduction method: High temperature retorting at 1500° F.


Speci f ic g rav i ty A . P . I , g rav i ty Sulfur , percent Nitrogen, percent Pour p o i n t , °F. Viscos i ty , S.U.

seconds at 100" F.

1.063 1.6

.76 3.08

below 5

. 62

Naphtha (F rac . 1-Light d i s t i l l a t e


(Frac. l l - l l i ) Residuum Loss

•7)

Volume, percent

30.1.

15 . U

18.3 25.9

2.0


Sp. g r . " A . P . I . 0.887 28.0

1.012 8.3

1.108 1.337

N i t r o g e n , p e r c e n t

1.30

3 .20

l u l l li.02


Distillation at 760 mm. Hg

Cut at- Per-Sum, per- Spec.

No. 1 2 3 li 5 6 7

•c. 50 75

100 125 150 175 200

•F . 122 167 212 257 302 3U7 392

cent

3.0 15.3

7.0 li.9 3.9 U.3

cent

3.0 18.3 25.3 30.2 3li . l 38.1;

grav.

0.81.7 .87U .879 .889 .911 .956

Analysis of-Naphtha

(Frac. 1-7), in percent

Light dist. (Frac. 8-10), in percent



Olefins Aromatics*

0.3 6.9

1 1

98

1.0 26.0

2 3 95

*Includes some sulfur and nitrogen compounds.

Distillation at liO 1 _Hg_ Vis, at 100° F. K.V., S.U., c.s. sec.

Frac. No.

Cut at-•C. °F. 150 302 175 3U7 200 392

Percent

6.9 3.9

Sum, percent

Gravity

1.3.0 1.9.9 53.8

Specific, 60°/60° F.

"A.P . I . , 60° F . 7TT 6.2 3.9


•C. below 25 below 25 below 25

9 10

1.017 1.028 1.01.5

11 12 13 111

225 250 275 300

1.37 li82 527 572

3.2 I1.6 ii.e 5.7

57.0 61.6 66. li 72 .1

,066 ,098 .118 ,129

1.2 below 25 11 .2 30 .6 28 .8 35.8 116.6 38.lt 2li l . l i

63 136 539

1115

Residuum 25.9 98.0 1.337

Carbon res idue of residuum, 61..2 pe rcen t ; carbon res idue of c rude , 20.9 pe rcen t .

13

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TABLE 4. (Cont.)


Rifle, Colorado, U.S.A. Union Oil Company retort


Specific gravity 0.9U5 A.P.I, gravity 18.2 Sulfur, percent .71 Nitrogen, percent 1.89 Pour point, °F. 75 Viscosity, S.U. seconds at 100° F. 280

Naphtha (Frac. 1-7 Light distillate

(Frac. 8-10) Heavy distillate

(Frac. ll-ll») Residuum Loss

Volume, percent tLJTT~

1U.3

31.7 18.0

.3


1/Nitrogen, ' A . P . I . percent -E5TF

Sp. g oTBl

.870

.922

.988

31 .1

22.0 11.7


PROPERTIES OF

DeK&lk County, Tennessee, U.S.A. Royster - Tennessee Valley Authority r e t o r t

CRUDE SHALE OIL

Speci f ic g rav i ty A . P . I , g rav i ty Sulfur , percent Nitrogen, percent Pour p o i n t , *F. Viscos i ty , S.U.

seconds at 100° F

Volume, percen t

1.005 Naphtha (Frac . 1-7) 6.0 9.3 Light d i s t i l l a t e 3.38 (Frac . 8-10) 21*.0

.88 Heavy d i s t i l l a t e below 5 (Frac . 11-Ut) 35.0

Residuum 33 .5 220 Loss 1.5


Sp. g r . "A .P . I . 0.853 31*.l*

.918 22 .6

.992 11 .1 1.101*

Ni t rogen , p e r c e n t

0 .22

. 3 1

.75 l . W *


Distillation at 760 mm. Hg

Frac. No.

Cut at-•C. "FT

Percent

"55" 75

100 125 150 175 200

122 167 212 257 302 31*7 392

Sum, per- Spec. cent gray.

0.1 2.6

0.1) 2.7) 0.823

Tar acids Tar bases Neutral oil: Paraffins and naphthenes

Olefins Aromatics*

Analysis of-Naphtha 1/Light dist.

(Frac. 1-7), (Frac.8-10), in percent in percent

15.9

21 55 21*

•Includes some sulfur and nitrogen compounds.


Distillation at 760 mm. Hg Sum,

Frac. Cut at- Per- per- Spec. No. 1 2 3 1* 5 6 7

•c. SO 75

100 125 150 175 200

• F . 122 167 212 257 302 3U7 392

cent

1.6 l*.t*

cent grav.

1.6 0.835 6.0 .860



Olefins Aromatics*

Analys is of— _ _ _ — . ^ Naphtha L igh t d i s t .

( F r a c . 1-7) , ( F r a c . 8 - 1 0 ) , in percent in percent

25 21 si*

175 1.6

5 17 78

•Includes some sulfur and nitrogen compounds

Frac. Cut at-No.

9 10

"C. Percent

150 302 3.3 175 3I47 6.0 200 392 5.0

11 225 U37 7.8 12 250 1*82 6.5 13 275 527 8.9 lit 300 572 11.5

Distillation at 1*0 mm. Hg Sum, percent

Residuum 1*8.0

6.0 12.0 17.0

2lt.8 31.3 1*0.2 51.7

99.7

Gravity Specific, 60°/60° F.

0.85k .869 .882

.891

.912

.930

.91:3

•A.P . I . , 60° F.

Anil ine point ,

"C.

Vis . a t 100° F.

3U.2 31.3 28.9

27.3 23.7 20.7 18.6

11.7

32.8 32.0 35.h

W)

(1 / )

K.V., c . s .

S.U. s e c .

7.7 13.7 2l».l 50 .1

51 72

115 230

9 10

11 12 13 111

Frac . No. 8

Cut a t -°C. °F. 150 302

Percent 5.1l

D i s t i l l a t i o n at ttO mm. Hg Sum, Gravity p e r - Spec i f ic , ' A . P . I . cent 60°/60° F. 60° F. 11.1* 0.895 26.6

An i l i ne p o i n t ,

•c. 10.0

Vis. a t 100° F. K.V. S.U. c . s . s e c .

175 31:7 200 392

225 250 275 300

Residuum

107 1*82 527 572

9.7 8.9

8.9 8.1, 7.7

10.0

33.5

21.1 30.0

38. 1,7. 55. 65.

98.5

• 913 .937

.961

.981, 1.003 1.018

1.101*

23.5 19.5

15.7 12.3

9.6 7.5

7.9 1*.0

1.7 .1*

- 1 . 2 1.6

8.1 18.3 1*1*.2

11,2.0

52 90

205 655

Carbon residue of residuum, _J_^_ percent ; carbon res idue of crude, 3.9 percent .

1/ This sample was run before these determinations were included in the method.

1*858

Carbon res idue of residuum, 20.3 pe rcen t ; carbon res idue of c rude , 7.5 p e r c e n t .

11* -

Source of shale: Eduction nethod:

Puertollano, Spain Pumpherston retort


Specif ic gravity A.P.I , gravity Sulfur, percent Nitrogen, percent Pour point, *F. Viscosi ty , S.U.

seconds at 100' F

0.895 26.6

.1)0

.68 70

5o

PHOPERTIES OF COMPOS ITE^RACTIONS

Naphtha (Frac. 1. Light d i s t i l l a t e

(Frac. 8-10) Heavy d i s t i l l a t e

(Frac. 11-Uj) Residuum Loss

•7)

Volume percent

13.8

25.2

1)2.0 18.0

1.0

Sp. gr. 'A.P.I . 0.792

.856

.915

.979

1)7.2

33.8

23.1 13.0

Nitrogen, percent

0.18

.38

.76 1.15


D i s t i l l a t i o n at 760 am. Hg ~~— "~ Sum?

Frac. Cut a t - Per- per- Spec. No. *C. *F. cent cent gray.

1 50 122 2 75 167 3 100 212 1) 125 257 5 150 302 6 175 31)7 7 200 392_

1.2 1.2 0.762 -U.7 5.9 -777 7.9 13.8 .806

Analysis of-



Olefins Aromaties*

Naphtha"" Light d i s t . (Frac. 1-7) , (Frac.8-10) , in percent in percent

1)2 1)2 16

2.

56 18 26

•Includes some sulfur and nitrogen compounds.

D i s t i l l a t i o n at 1|0 mm. Hg

Frac. No.

Cut a t -*C. *F.

Percent

Sum, percent

Gravity Specific, 60 7 6 0 * F.

•A.P.I. , 60* F.

Aniline point, •c.

Vis. at 100' F. I.V., c.s.

S.U.. sec.

9 10

11 12 13

150 302 175 31)7 200 392

225 250 275 300

U37 1)82 527 572

7.2 9.2

8.9 10.0 10.3 12.8

21.0 30.2 39.0

1)7.9 57.9 68.2 81.0

Residuum 18.0 99-0

0.81)1 .851. .870

.930

.936

.979

36.8 31).2 31.1

28.1) 26.1 20.7 19.7

13.0

1)5.1) 1)5.8 50.2

55.0 58.U 63.2 68.li

5.9 9.6

16.6 31.2

1)5 58 83

UiS

Carbon residue of residuum, lull percent) carbon residue of crude, 0.9 percent.

U858

4. (Cont.)


Boksburg, Transvaal, Union of South Africa Salermo retort


Speci f ic gravity A.P.I gravity Sulfur, percent Nitrogen, percent Pour point, *F. Viscos i ty , S.U.

0.906 21).7

.a,

.85 55

Naphtha (Frac. 1-7) Light d i s t i l l a t e


(Frac. 11-11)) Residuum

Volume percent

19.1

16.9

32.1 31.8


Sp. gr. 'A.P.I . 0.773 51.6

.861) 32.3

• 921» 21.6 1.000 10.0

N i t rogen , percent

0.1k

. 50

.85 1.30

seconds at 100' F. 63 Loss .1


Distillation at 760

Frac. No.

1 2 3 h 5 6 7

Cut *C. 50 75

100 125 ISO 175 200

a t -•F . 122 167 212 257 302 3U7 392

Percent

1.8 2.9 3 .1 /4.0 7.3

Sum, percent

1.8 l).7 7.8

11.8 19.1

Spec. grav.

0.709 .735 .756 .779 .808

Analysis of Naphtha Light d i s t .

(Frac. 1-7), in percent

(Frac. 8 - 1 0 ) , in percent

Tar acids Tar bases Neutral o i l )


Olefins Aromatics*

1.8 . 6

37 1)8 15

5.3 7.6

32 Uo 28

•Includes some sul fur and nitrogen compounds.

Frac. No.

Out a t -•C. 'F.

Percent

D i s t i l l a t i o n at 1)0 mm. Hg Sum, Gravity per- Specif ic , "A.P.I, cent 6076c-' F. 60' F.

Anil ine point ,

•c.

Vis . a t 100" F. K.V., S .D. , c . s . s e c .

9 10

11 12 13 11)

150 302 175 31»7 200 392

225 250 275 300

1.37 U82 527 572

Residuum

6.7 5.3 U.9

6.5 6.6 8.0

11.0

31.8

25.8 31.1 36.0

1)2.5 1)9.1 57.1 68.1

99.9

0.8U5 .872 .883

.897

.907

.931 •9l)li

1.000

36.0 30.8 28.8

26.3 21).5 20.5 18.1)

10.0

36.0 1)3.0 1)7.0

50.1) 51 .0 5 3 . 0 50.U

6 .6 10.6 19.6 1)0.5

U8 61 96

190

Carbon residue of residuum, 7.1 percent; carbon residue of crude, 2.5 percent .

15

http://68.li

TABLE 4. (Cont.)

Source of shale : Eduction method:

Glen Sar i s , N.S.W., Australia Modified Pumpherston retort


Speci f ic gravity 0.888 A.P.I , gravity 27.9 Sulfur, percent .56 Nitrogen, percent .52 Pour point , °F. 60 Viscos i ty , S.U.


s e c o n d s at 1 0 0 ° F. SU

Naphtha ( F r a c . 1-Light d i s t i l l a t e


(Frac. 11-lli) Residuum Loss

•7)

Volume > percent

Ui.6

20.1:

37.1 27.2

Sp. gr. 0.782

.81(6

.898

.956

• A . P . I .

1:9.5

35.8

26.3 16.5

Nitrogen, percent

0.10

.21:

.50

.81



Analysis of—

Frac. No.

Cut a t -'57 *F.

Percent

percent

Spec. gray.

Naphtha Light d i s t . (Frac. 1-7), (Frac. 8-10) , in percent in percent

50 75

100 125 150 175 200

122 167 212 257 302 3U7 392

2.3 1».5 7.8

2. 6.

1U.

0.753 .771 .796



Olefins Aroma t i c s *

ii5 ii3 12

1.0 37 23


Frac. No.

Cut a t -rC. "F."

Percent

D i s t i l l a t i o n at 1:0 mm. Hg Sum, Gravity Aniline per- Specif ic , "A.P.I., point, cent 6o/60' F. 60' F. °C.

Vis . at 100" F. K.V., S.U., c . s . s e c .

9 10

11 12 13

150 302 175 3U7 200 392

7.1: 22.0 6.3 28.3 6.7 35.0

225 250 275 300

1:37 U82 527 572

7.8 8.5 9.0

11.8

1:2.8 51.3 60.3 72.1

Residuum 27.2 99.3

0.830 .81:8 .861

.876

.887

.901:

.915

.956

39.0 35.1: 32.8

30.0 28.0 25.0 23.1

16.5

1:6.2 1:9.2 50.0

57.2 57.8 62.0 66.0

5 .6 9 .1

15.3 1:7.3

kh 56 79

220


Kvamtorp, Sweden Roekesholm retort


Speci f ic gravity A.P.I , gravity Sulfur, percent Nitrogen, percent

0.977 13.3

1.65 .68

Pour point, - F. below 5 Viscos i ty , S.U.

seconds at 100' F. 77

Naphtha (Frac. 1-7) Light d i s t i l l a t e


(Frac. 1 1 - U J ) Residuum Loss

Volume, percent

16.5

2U.7

35.1 22.8

.9


SP- P.: 0.818

.926

1.006 1.099

FRACTIONS Nitrogen,

"A.P.I. percent 1:1.5 0 .17

21.3 .30

9 .2 .62 .97

DISTILLATION AMD ANALYTICAL DATA

D i s t i l l a t i o n at 76c

Frac. Cut a t - Per-No. *C. '?. cent

1 mm. Hg Syim)

per- Spec. cent grav.

Analysis of-Naphtha Light dist.

(Frac. 1-7), (Frac. 8-10), in percent in percent

50 75

100 125 150 175

122 167 212 257 302 31:7

2.0 3.3 U.6

2.0 5.3 9.9

.773

.785

.818 200 392 6.6 16.5 .81:9



Olefins Aromatics*

2l» 35 111"

1».3 5 . 2

3 16 81

*Includes some sulfur and nitrogen compounds.

Frac. No.

Cut a t -•C. "F.

Percent

D i s t i l l a t i o n at UO mm. Hg Sum, Gravity Aniline per- Specif ic , A.P.I . , point, cent 60°/60' F. 60" F. *C.

Vis. a t 100° F. K.V., S.U., c . s . s e c .

9 10

11 12 13 Ik

150 302 175 31:7 200 392

225 1:37 250 1:82 275 527 3 0 0 572

7.6 8.3

6.9 8.3 8 .1

11.8

21:. 1 32.1: 1:1.2

1:8.1 S6.ii (k.S 76.3

0.891: .926 .955

.976

.991: l.OOii 1.033

26.8 21.3 16.7

13.5 10.9

9.1: 5.5

Below 0 Below 0 Below 0

Below 0 10.0 Below 0 22.7 Below 0 65.8 Below 0 352.1:

60 110 305

1630

Carbon residue of residuum, 3.0 percent; carbon residue of crude, 0.9 percent. Residuum 22.8 99.1 1.099

Carbon residue of residuum, 11.8 percent; carbon residue of crude, 3 . 0 percent .

U858 16

Source of shale i Kvarntorp, Sweden Eduction method! LJungstrom process

PROPERTIES OF CHTOE SHALE OIL

Speci f ic g rav i ty A . P . I , g rav i ty Su l fur , percent Ni t rogen, percent

0.809 ii3.lt

. 71

.11 Pour p o i n t , *F. below 5 Viscos i ty , S.U.

seconds at 100" F. 29

Naphtha (Frac . 1-Light d i s t i l l a t e

(Frac . B-10) Heavy d i s t i l l a t e

(Frac . 11-lU) Residuum Loss

•7)

Volume, percent

76.8

20.8

1.3 .3 .8

PROPER' COMPOSITE

Sp. gr . 0.783

.893

.951

TIES OF FRACTIONS

•A.P . I . 1.9.2

27.0

17.3

Ni t rogen, percent

0.07

.13

.20


D i s t i l l a t i o n a t 760

Frac . Cut a t - Per-No. 'C. "F. cent

mm. Hg Sum, p e r - Spec. cent grav.

50 122 75 167 2.2 100 212 6.6 125 257 16.3 150 302 21.6 175 31*7 16.8 200 392 13.3

2.2 8.8

25.1 I46.7 63.5 76.8

0.668 .706 .7lt7 .783 .820 .836

Analysis of —



Olefins Aromatics*

Naphtha Light d i s t . (Frac. 1-7), (Frac . 8-10) , in percent in percent

0.1. .2

63 11 26

.3 3 .1

5 30 65

Încludes some su l fur and n i t rogen compounds.

D i s t i l l a t i o n at liO mm. Hg

8 9 10

11 12 13

m

Frac . No.

Cut a t -•C. "F.

Percent

Sum, p e r cent

Gravity Spec i f ic , "A.P.I . , 60*/60* F. 60* F.

Anil ine po in t ,

•c

Vis. a t 100* F. K.V., S.U., c . s . s ec .

150 302 175 3U7 200 392

225 1(37 250 U82 275 527 300 572

12.5 5.9 2.1t

89.3 95.2 97.6

1.3 98.9

0.877 .912 .932

.951

29.9 23.7 20.3

17.3

.6 2.8

.8

Residuum .3 99.2

1*858

4. (Cont.)


Scotland Pumpherston retort




0.87U 30.1*

.35

.77 75

Naphtha (Frac.1-7) Light distillate (Frac.8-10)

Heavy distillate (Frac.11-lh)

seconds at 100 °F. 1*8 Residuum Loss

Volume, percent

19.5

19.1*

3li.lt 25.1 1.6

S p . g r . 0.756

•A .P . I . "1577-

.81*7 35.6

.891 27.3

.968 11*.7


0 .13

.1*3

.82 1.28



Frac . No.

1

Cut 4C. 50

a t -*F. 122

a t 760

Percent

mm. ] Sum, pe r cent

lg

Spec. grav.

Analysis of~

75 100 125 150 175 200

167 212 257 302 31.7 392

1.1* 3.7 7.3

11.8 15.0 19.5

0.699 .716 .735 .755 .777 .796



Olefins Aromatics*

Naphtha L igh t d i s t . ( F r a c . 1 -7) , ( F r a c . 8 - 1 0 ) , i n percen t i n p e r c e n t

1.2

!»7 1.3 10

2T0~ 2 .6

36 36 28

ttlncludes some sul fur and n i t r ogen compounds.

D i s t i l l a t i o n at 1.0 JiS_

Frac . No.

Cut a t -~*F7

"T5iT 302 175 31.7 200 392

Percent

Sum, pe r cent

Gravity Specif ic , 60 7 6 0 ' F.

'A.P. I . , 60* F.


°C.

Via a t 1 0 0 ' F. K.V., s.tr.

s e c .

9 10

11 12 13 U*

6.7 7.5

21*.7 31.1* 38.9

225 1*37 7.5 1*6.1* 250 1*82 5.1* 51.8 275 527 8.8 60.6 300 572 12.7 73-3

Residuum 25.1 98.1.

0.832 .81.1 .863

.873

.889

.893

.902

.968

3 0 ~ 36.8 32.5

30.6 27.7 27.0 25.1.

11..7

T O " 50.8 56.2

60.2 66 .8 73.6 77.6

5.8 12.5 12 .8 25.6

1*5 68 69

120

Carbon res idue of residuum, l*.l* pe rcen t ; carbon res idue of c rude , 1.2 p e r c e n t .

17 -

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http://3li.lt

http://Sp.gr

TABLE 4. (Cont.)



Specif ic g rav i ty A .P . I , g rav i ty Sul fur , percent Nitrogen, percent Pour p o i n t , "F. V i scos i t y , S.U.

Autun, France Pumpherston r e t o r t

0.931 20.5

.51

.90 65



(Frac .11- lb) Residuum


Severac, France Harecaux retort

seconds at 100°F. 87 Loss

Volume, percent

2.3

21*.9

U3.6 28. l i

.8


Sp.gr . O.B29

.868

.91u

.999

FRACTIONS

•A .P . I . 39.2

31.5

23.3 10.1

Nitrogen, percent

O.bO

.58

.85 1.36


Specif ic g rav i ty A .P . I , g rav i ty Sul fur , percent Nitrogen, percent Pour p o i n t , °F. Viscos i ty , S.U.

seconds at 100°F.

0.925 21.5

3.00 .53

30

1*5

Naphtha (Frac .1-7) Light d i s t i l l a t e


(Frac.11-11.) Residuum Loss

Volume, percent

23.5

25.7

31.0 19.2

.6


0.807 1.3.8

.896 26.1.

.961. 15.3 l.oU* 1..0

Ni t rogen , Dercent

0.15

.35

.65 l.Ol.

DISTILLATION AND ANALYTICAL DATA DISTILLATION AND ANALYTICAL DATA


Frac . No.

Cut

•c a t -•F .

a t 760

Percent

mm. Sum, percent

Hg

Spec, grav.

Analysis of-

50 122 75 167

100 212 125 257 150 302 175 31.7 200 392 2.3 2.3 0.829



Olefins Aromatics*

Naphtha!/ (Frac. 1-7), in percent

Light d i s t . (Frac . 8-10) , in percent

33 36 31

*Includes some sulfur and n i t rogen compounds.

D i s t i l l a t i o n at 1.0

Frac. No.

Cut a t -*C. «F.

Percent

Sum, p e r cent

Oravity _HfL

9 10

11 12 13 11.

Residuum

150 302 G73 575" 175 31.7 10.6 17.2 200 392 10.0 27.2

Specif ic, 6 0 7 6 0 ° F .

225 250 275 300

137 1.82 527 572

10.9 11.5 10.7 10.5

38.1 1.9.6 60.3 70.8

28.1. 99.2

0.851. .861. .878

.890

.908

.922

.939

.999

M . P . I . , 60" F.

Anil ine point,

°C. 35.2 32.3 29.7

27.5 2l*.3 22.0 19.2

10.1

T57T U3.2 1*5.1

1*9.8 53.2 55.1* 58.6

Vis , a t 100° F. K.V., c . s .

S.U. sec .

6.2 11.7 2U.li 63.2

1.6 61*

115 290

D i s t i l l a t i o n at 760 mm. Hg

Frac. Cut a t - Per-

Frac. No.

9 10

11 12 13 11*

Sum, Per- Spec.

Analysis of-Naphths. L igh t d i s t .

(F rac . 1-7) , ( F r a c . 8 - 1 0 ) , No.

1 2 3 1* 5 6 7

4C. 5o 75

100 125 150 175 200

*F. 122 167 212 257 302 31*7 392

cent

0.9 3.5 5.6 6.0 7.5

cent

0.9 l*.l*

10.0 16.0 23.5

grav.

0.733 .761* .790 .818 .81*0



Olefins Aromatics*

i n pe rcen t 1.6

.1*

31 1*1 28

i n pe rcen t 1.6 2.1*

28 21* 1*8

*Includes some s u l f u r and n i t r ogen compounds.

D i s t i l l a t i o n at 1*0

Cut a t -*c7—"FT

175 200

225 250 275 300

Per cent

Sum, p e r cent

Gravi ty Jfc_

302 31*7 392

1*37 1*82 527 572

~ T ^ 3675" 10.7 1*1.2 8.0 1*9.2

Specif ic , 6 0 V 6 0 ' F .

58.3 6 u . l 70.9 80.2

Residuum 19.2 89.1*

787T .895 .917

.936

.957

.973

.989

1.01*1*

•A.P . I . 60° F.

30.1* 26.6 2?.e

19.7 16.1* 13.9 11.6

li.O

Aniline point,

•c.

Vis, at 100* F. K.V.,

21*.0 21*.8 26.2

27.1 27.6 28.2 28.9

S.U. sec.

7.6 ll*.6 27.2 79.0

51 76

130 360

Carbon residue of residuum, 6.7 percent) carbon residue of crude, 2.0 percent.

1/ Insufficient sample for analysis.

1*858


18 -

http://Sp.gr

TABLE 4. (Cont.)


Severac, France Cantieny retort


St. Hilaire, France Lantz retort



seconds at 100 °F

0.959 Naphtha (Frac.1-7) 16.0

3.1)0 .65

below 5

as

Light d i s t i l l a t e (Frac. 8-10)

Heavy d i s t i l l a t e (Frac. 11-11))

Residuum Loss


Volume, percent

27.9

25.0

26.7 19.1)

1.0

§Ei 0.838

. .918

1.001 1.099

°A.P.I . 37.1)

22.6

9.9

Nitrogen, percent

0.16

.37

.81 1.11)



Frac. Cut a t - Per- p e r - Spec. No. 'C. *F. cent cent grav.

Analysis of-

75 100 125 i5o 175 200

T2T" 167 212 257 302 31)7 392

2.9 5.9 12.0 19.1) 27.9

.789

.812

.827

.81)6

.861)


Paraffins and

naphthenes Olefins Aromatics*

Naphtha Light dist. (Frac. 1-7), (Frac.8-10), in percent in percent

25 22

53

21) 18 58


Frac. No. 8

Cut a t -•C. °F. 150 302

Percent 8.5

D i s t i l l a t i o n a t 1)0 mm. Hg Sum, Gravity per - Specif ic, "A.P.I., cent 60°/60° F. 60° F. 36.1) O.H98 26.1

Aniline point ,

•c. llt.l)

Vis . a t 100° F. K. V., S. U.,

c . s . s ec .

9 10

11 12 13 11)

175 31)7 8.1t 1)1).8 200 392 8.1 52.9

225 250 275 300

1)37 1)82 527 572

7.8 5.6 6.5 6.8

60.7 66.3 72.8 79.6

.917

.91)1

.962

.993 1.012 1.01)0

22.8

18.9

15.6 11.0

8.3 h.6

17.0 20.0

21.9 18.2 28.6 30.8

7.1) 15.1) 35.9

107.2

50

79 165 1)90

Residuum 19.1) 99.0 1.099


Speci f ic g rav i ty A.P . I , g rav i ty Sulfur , percent Nitrogen, percent Pour p o i n t , °F. Viscos i ty , S.U.

seconds at 100 °F.

D i s t i l l a t i o n a t

Frac . No.

1 2 3 1) 5 6 7

Frac. No.

Cut a t -°C. °F. 50 122 75 167

100 212 125 257 150 302 175 31)7 200 392

Cut a t -°C. °F.

8 150 302 9 175 31)7

10 200 392

11 225 1)37 12 250 1)82 13 275 527 111 300 572

Residuum

Carbon res idue of

0.908 21).3

.61

.51) 60

5o

, 760 mm.

Naphtha Light di

(Frac. Heavy d^

(Frac, Residuur Loss

DISTIL LAT]

Hg Sum,

Per- p e r - Spec. cent cent grav.

3.2 3.2 0.71)1) 1).9 8.1 .766 5.5 13.6 .790 6 .1 19.7 .822

Dis t i ]

Percent £.9 8.8 7.3

8.1 8.6 8.3

lO.U

21.5

residuum

Sum, p e r - £ cent t 25.6 31).1) 1)1.7

1)9.8 58.1) 66.7 77 .1

98.6

, 8.1)


Volume, percent Sp. g r . "A.P. I .

(Frac.1-7) 19.7 0.786 1)8.5 L s t i l l a t e .8-10) 22.0 .87li 30.1) L s t i l l a t e .11-11)) 35.1) .938 19.1) 0 21.5 1.023 6.8

1.1)

[ON AND ANALYTICAL DATA

Analysis of —



Olefins Aromatics*

Încludes some

Llation at 1)0 mm. Hg Gravity

Specific, °A.P. I . , >0°/60° F. 60° F. 0.862 32.7

.871 31.0

.888 27.9

.909 21).2

.921) 21.6

.91)3 18.6

.968 1U.7

1.023 6.8

percent ; carbon res:

Naphtha ( F r a c . 1 - 7 ) ,

in percent 2.0 2.0

37 1)7 16

su l fur and n i t rogen

Anil ine Vis . a t point , K.V.

°C. c . s . 39.? 1)0.1) 1)1.8

1)2.6 6.1) 1)9.2 11.2 52 .9 21.2 53.8 58.2

idue of crude, 2.


0 . 1 1

.27

.53 1.20

L i g h t d i s t . ( F r a c . 8 - 1 0 ) , i n p e r c e n t

Lo 2.h

25 1)1 31)

compounds.

100° F. S.U. s e c .

1)7 63

105 270

0 p e r c e n t .


1*858 - 19 -

CONCLUSION

A standardized analytical procedure for the examination of crude shale oil is presented. The method is an adaptation of the Bureau of Mines crude-petroleum method. The proposed method considers the relative instability of shale oil toward heat and its high content of unsaturated hydrocarbon, nitrogen, oxygen, and sulfur compounds.

Results obtained by applying the method to 10 shale oils produced in the United States and to 10 shale oils from foreign countries are presented.

U858 - 20

Int. - Bu. of Mines, Pgh., Pa.

Documents

ANALYSIS OF CRUDE SHALE OIL - University of Utahrepository.icse.utah.edu/dspace/bitstream/123456789/6842/1/Anal of... · ANALYSIS OF CRUDE SHALE OIL by ... John S., Analytical Distillation