SPECIFIC GRAVITY DETERMINATION OF MARINE SEDIMENTS Joseph C. Henderson United States Naval Postgraduate School THESIS SPECIFIC GRAVITY DETERMINATION OF MARINE SEDIMENTS by Joseph C . Henderson April 1970 TkLt> document kat> bzen app>wve,d ^oa. pubLLc Ke.- Iza^e. and 6 ale.; i£t> di6Vu.bation l& unturuAzd. T133476 Specific Gravity Determination of Marine Sediments by Joseph C. Henderson Lieutenant Commander { United States Navy B.S., United States Naval Academy, 1959 Submitted in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE IN OCEANOGRAPHY from the NAVAL POSTGRADUATE SCHOOL April 1970 ABSTRACT Accurate specific gravity measurements are required for the analysis of physical properties of marine sediments. Application of the bottle pycnometer technique, the standard determination method, is time- consuming, tedious, and perhaps subject to inaccuracies in the case of fine particulate matter. A review of methods currently in use was con- ducted to ascertain the present state of the art and reveal any new developments in this field. Specific gravity values for three operating modes of the air comparison pycnometer, two of which use helium, were compared with bottle pycnometer values for four test materials. The air comparison pycnometer determinations, regardless of operating mode, resulted in higher specific gravities than their counterpart bottle pycnometer values for kaolinite , montmori llonite , and marine sediment samples. The use of helium as the comparison medium in the air com- parison pycnometer appears to reduce the surface active characteristics of the colloidal material. Specific gravity determinations by all four test methods agreed very well for powdered quartz samples with a known specific eravitv. _^^_^_^_ LIBRARY IAVAL POSTGRADUATE SCHOOL MOHTEREY, CALIF. 93940 TABLE OF CONTENTS I. INTRODUCTION . . 9 SPECIFIC GRAVITY AS A PHYSICAL PROPERTY OF MARINE SEDIMENTS ... 10 BASIC SPECIFIC GRAVITY DETERMINATION L1 PURPOSE OF THIS INVESTIGATION 12 II. REVIEW OF METHODS CURRENTLY IN USE 14 ACADEMIC INSTITUTIONS ,, 14 MANUFACTURING AND DISTRIBUTION FIRMS 15 LABORATORIES AND PRIVATE INDIVIDUALS 15 DISCUSSION OF RESULTS 16 III. PROCEDURES FOR SPECIFIC GRAVITY DETERMINATION 17 BOTTLE PYCNOMETER METHOD 17 AIR COMPARISON PYCNOMETER 23 JOLLY BALANCE 35 BERMAN DENSITY BALANCE 40 DIFFERENTIAL GRAVITY TUBE 44 DERIVED EQUATION FOR SPECIFIC GRAVITY COMPUTATION 47 IV. COMPARISON OF AIR COMPARISON PYCNOMETER AND BOTTLE PYCNOMETER METHODS 50 GENERAL 5o SAMPLE PREPARATION 54 SPECIFIC GRAVITY RESULTS FOR KAOLINITE 57 SPECIFIC GRAVITY RESULTS FOR MONTMORILLONITE 61 SPECIFIC GRAVITY RESULTS FOR QUARTZ 65 SPECIFIC GRAVITY RESULTS FOR SEDIMENT CORE 67 V. CONCLUSIONS AND RECOMMENDATIONS 72 APPENDIX A - Copies of Review Correspondence 75 APPENDIX B - Summary of Review Comments . 79 APPENDIX C - Derivation of an Equation Relating Specific Gravity, Bulk Wet Density, and Water Content 90 APPENDIX D - Computer Program 93 APPENDIX E - Computer Output for NCEL Data 95 APPENDIX F - Computer Output for Hydrographic Office Data .... 109 APPENDIX G - BIMED Analysis Results 116 BIBLIOGRAPHY 122 INITIAL DISTRIBUTION LIST 124 FORM DD 1473 125 LIST OF TABLES Table Page I Results of specific gravity determinations 58 of ten samples of kaolinite II Results of specific gravity determinations 62 of ten samples of montmori llonite III Results of specific gravity determinations 66 of twelve samples of quartz IV Results of specific gravity determinations 70 of eight alternate intervals of a 50 inch core sample LIST OF FIGURES Figure Page 1 Calibration Curve for 100 Milliliter Pycnometer 20 Bottle 2 Schematic of Beckman Model 930 Air Comparison 25 Pycnometer 3 End View of Air Comparison Pycnometer 27 Showing Handwheels 4 End View of Air Comparison Pycnometer 28 Showing Sample Cup Compartment 5 Side View of Air Comparison Pycnometer 29 Showing Differential Pressure Indicator and Digital Volume Counter 6 Kraus Jolly Balance 36 7 Berman Density Balance 41 8 Bottle Pycnometer Equipment 51 9 Air Comparison Pycnometer with Vacuum Pump, 51 Helium Bottle and Regulator 10 Quartz Crushing Apparatus 56 11 Quartz Crusher Components 56 12 Plot of Specific Gravity Determinations on 60 Kaolinite 13 Plot of Specific Gravity Determinations on 64 Montmorillonite 14 Plot of Specific Gravity Determinations on 68 Quartz 15 Plot of Specific Gravity Determinations on 71 Sample Core ACKNOWLEDGEMENTS Appreciation is expressed to Dr. R. J. Smith for suggesting this thesis topic and for his advice and encouragement throughout its development. Gratitude is also extended to the Naval Facilities Engineering Command for their interest in and support of the marine sediment research program at the Naval Postgraduate School. I. INTRODUCTION Specific gravity by strict definition is the ratio of the mass of a given volume of a substance, at a stated temperature, to the mass of an equal volume of a reference substance, at a stated temperature [Thewlis, 1962]. It is common practice in soil engineering to use weight in place of mass in this definition, where weight is a force equal to the product of mass and the acceleration of gravity. In the case of marine sediments the specific gravity is usually referred to an equal volume of distilled water at 4 C . The above definition allows the expression of three different forms of specific gravity. These are 1) the specific gravity of solids, G , 2) the apparent specific gravity, G , and 3) the bulk specific gravity, a. G . The specific gravity of solids is the ratio of the weight in air m of a given volume of soil solids, exclusive of voids or impermeable pore spaces, at a stated temperature, to the weight in air of an equal volume of distilled water at 4 C. Apparent specific gravity is the ratio of the weight in air of a given volume of soil solids plus the voids and pore spaces normal to the material, at a stated tempera- ture, to the weight in air of an equal volume of distilled water at 4 C. The bulk specific gravity is the ratio of the weight in air of a given volume of a permeable material (including material solids, impermeable voids or pores, and interstitial spaces between adjacent particles), at a stated temperature, to the weight in air of an equal volume of dis- tilled water at 4 C. The specific gravity of solids applies to fine particulate matter, and is a parameter frequently determined in the analysis of the physical properties of marine sediments. The other two forms of specific gravity are usually related to coarser material and are used in other aspects of soil mechanics practice [Office of Chief of Engineers, 1965]. The specific gravity of solids is synonymous with the terms absolute, true, or real specific gravity. Unless otherwise modified, the term specific gravity will here refer to the specific gravity of solids. Specific gravity is a measure of, and a means of expressing, the relative heaviness of a material. The density of a marine sediment is defined as the weight per unit volume, and it is a measure of its denseness. Density is synonymous with the terms unit weight and specific weight, and is usually expressed in units of pounds per cubic foot or grams per cubic centimeter, whereas specific gravity is a unitless ratio. Dry density is directly proportional to specific gravity, if the relative volumes of solid particles and void spaces are maintained constant. Specific Gravity as a Physical Property of Marine Sediments The specific gravity can be used as a very precise index property for Che identification of minerals. The specific gravity of a marine sedi- ment represents the weighted average of the specific gravities of all the various mineralogic constituents of the sediment. The specific gravii these constituents may vary widely. Gypsum has a specific ivity of about 2.3, whereas hematite has a specific gravity of 5.3. Th< tee in ledimenta of quartz, with a specific gravity of 2.65, an'i the ochex illicate minerals, usually narrows the range of ledimenta to values between 2.5 to 2.9. Some 10 marine sediments are rich in calcium carbonate and would exhibit higher specific gravity values. The value of the specific gravity is applied to several other cal- culations in the analysis of the physical properties of marine sediments Its accuracy is of great importance in calculations of parameters such as void ratio, porosity, saturated void ratio, and sub-sieve grain size distribution. basic Specific Gravity Determination For a relatively large solid body the specific gravity is simply the weight of the body divided by the weight of an equal volume of water. Its determination is a three step procedure. First, the object is weighed. Next, the weight of an equal volume of water is determined. And finally, the weight of the object is divided by the weight of the equal volume of water. Determining the weight of the solid body presents no significant problem. Accurate determination of the volume of a solid is considerably more difficult. Twenhofel and Tyler [1941] indicate four basic methods are available for determining the specific gravity of a solid. The volumetric method is appropriate if the solid body has a simple geometrical shape. The dimensions of the object are carefully mea- sured, its volume calculated, and then the weight of an equal volume of water obtained. The hydrostatic method incorporates the use of Archi- medes principle to experimentally determine specific gravity. This principle states that the buoyant force on an immersed body is equal to the weight of the liquid displaced by the body. A direct volume measurement of the object is not made as the loss of weight of the 11 object in water represents the desired weight of an equal volume of water . A third procedure for determining specific gravity is the flotation method, in which the specific gravity of a solid object is compared directly with a liquid of known specific gravity. When the solid will neither sink or rise in a liquid the specific gravity of the solid is the same as that of the liquid. The fourth method is the direct dis- placement method. A flask is filled with distilled water of determined temperature to a given volume mark and the flask is weighed. The sample is then added to the flask and the new volume and weight is noted. The specific gravity equals the difference in weights divided by the dif- ference in volumes. Purpose of this Investigation The specific gravity determination is relatively easy for a larger iid body. Marine sediments are colloidal, however, and the appli- cation of the above methods requires considerations that complicate the rminat : m lignif icant ly . The volumetric method involves the problem • mining the volume of fine particulate matter. A sample of marine Ltnent c I ; of very fine grained particles with voids and inter- tilial passages that make this determination extremely difficult. • .tic weighting method and the displacement method ' ill the air is removed from the sediment Lied water to ensm. th.it the water is displaced il. A I i thesi method ire detailed attenti on imp Le . 12 The bottle pycnometer technique, which is an application of the hydrostatic weighing procedure, is considered the standard method for the specific gravity determination of soils and sediments. Application of this method is tedious, time consuming, and is of questionable accuracy in some cases. The results for sands and silts are believed to be accurate. Bottle pycnometer values for fine particulate material, such as clays, may be erroneous, but are usually consistent with strict adherence to the procedures. Incomplete air removal from the suspended sediment is the primary source of error and results in low specific gravity values. It is desirable to find a new and less time consuming specific gravity determination method and evaluate its accuracy and application with regard to marine sediments. 13 II. REVIEW OF METHODS CURRENTLY IN USE .on A review was made to determine the specific gravity determinate methods presently being used throughout the technical fields, and to discover if any new methods were under development. A total of 327 letters were sent to selected academic institutions, manufacturing and distribution firms, soil mechanics and marine research laboratories, and individuals known to be working in the field of interest. The inquiries to academic institutions, laboratories, and private individuals consisted of a covering letter indicating the purpose of the correspondence to- gether with a check - off type of questionnaire. Information was requested concerning the method, type of equipment, and accuracy of the specific gravity technique as utilized by the recipient. Sample copies of the covering letter and questionnaire are included in Appendix A. The commercial firms were asked for information concerning specific sanation equipment applicable to fine particulate solids. A copy of the letter to these firms is also included in Appendix A. 1 from 62 percent of these inquiries. nhi 1 1 I iv, t j t ut ions Tn< departments of chemistry contacted indicated that no ted in the area of specific gravity deter- atter. Of the 73 departments of geology ■'■ lndi< i ivity determinations were routinely Balance, bottle pycnometer, and i < i vi 1 engineering responded Lth th( ttle pycnometer mel hod as I hei c choice of 14 a specific gravity determination technique. When dealing with soils and clays twenty-three schools used this method while only one school used the air comparison pycnometer for the specific gravity determinations Three-quarters of the 34 departments of oceanography contacted answered the questionnaire, but only five of these indicated they were making analyses of marine sediments. Two use cylinders of a known volume plus the weight of the sample to determine wet density, two use the bottle pycnometer method, and one uses the air comparison pycnometer. A sum- mary of institutions who responded annotated by comments of interest is included in Appendix B. Manufacturing and Distribution Firms A total of 72 companies were contacted. Six companies manufacture balances which are specifically designed for or may be modified to determine specific gravity using the hydrostatic weighing technique. Most notable of these are the Berman Density Balance and the Kraus Jolly Balance. Four other firms manufacture or distribute density gradient column systems which may be used for specific gravity deter- mination. One firm manufactures a precision pressure gauge which can be installed in a system to determine the volume of a unknown sample size, and as such basically serves as the null pressure indicator in an air comparison pycnometer system to be described later. A summary of review results from the commercial firms may be found in Appendix B. Laboratories and Private Individuals Of the individuals and facilities sent questionnaires, six were using the bottle pycnometer method and three the air comparison pycno- meter. Other replies indicated application of flotation methods, 15 hydrostatic weighing methods, or bulk density measurements using a cylinder of known volume. Appendix B contains more detailed information concerning replies from laboratories and private individuals. Discussion of Results This review confirmed that the bottle pycnometer is the primary method now in use for making specific gravity determinations of fine particulate materials such as sediments. Although some replies indi- cated that extreme accuracy was not required for their particular effort, the accuracy stated by most of the users of the bottle pycnometer techni- que was + 0.005 to + 0.01. Those interested in precise and reproducible readings emphasized the care required to de-air the sample and to main- tain an adequate temperature control. To achieve desired accuracy one group evacuated the sample for 24 to 48 hours while continuously agi- tating the sample on a vibrating table. In another case a laboratory makes duplicate specific gravity determinations on two samples of a material and accepts the results if the values agree within + 0.01. Unfortunately no new techniques for the specific gravity deter- mination of fine particulate material were uncovered. It was noted, in general, that those using the gas pycnometer were unsure of the accuracy of their results and for the most part did not use helium as comparison medium. A majority of the replies indicated an interest in the results of the Naval Postgraduate School effort. 16 III. PROCEDURES FOR SPECIFIC GRAVITY DETERMINATION Standard procedures for analysis of the physical properties of marine sediments have not yet been established. Most of the techniques in use are modifications of those used in soil mechanics. The present study has revealed that five methods are in use for specific gravity deter- mination. These procedures are summarized here in some detail. The bottle pycnometer method and the air comparison pycnometer method, both of which are utilized for a comparative analysis in this paper, are presented in as much detail as could be obtained. The other methods are less strenuously treated with regard to operating procedure, however the advantages and disadvantages of all methods are discussed in con- nection with their applicability to marine sediments. Bottle Pycnometer Method This method is considered the standard for determining the specific gravity of soils, clays, and sediments. The loss of weight of the sample when immersed in water is obtained, and as such represents a variation of the hydrostatic weighing technique. The following pro- cedure was extracted primarily from Lambe [1959] and A.S.T.M. [1964]. 1 . Apparatus Required a. Pycnometer - volumetric flask of 100 or 500 milliliter capacity, or stoppered bottle of at least 50 milliliter capacity. b. Balance - sensitive to 0.01 grams if volumetric flask used, or 0.001 grams if stoppered bottle is used. c. Distilled water d. Vacuum source (optional) 17 Heat source - burner or hot plate Drying oven - capable of maintaining 105 C + 5 C temperature, g. Desiccator h. Thermometer - graduated to 0.1 C. Evaporating dishes. Medicine dropper or pipette. 2 . Calibration of Pycnometer For every specific gravity determination the weight of the pycnometer filled to the calibration mark with distilled water at the test temperature is required. A calibration curve for each pycnometer may be plotted, which allows this value to be obtained graphically for any test temperature. a. The thoroughly cleaned and dried pycnometer is weighed, and the weight is recorded (Wf ) . The cleaning procedure requires washing with glassware cleaner, rinsing with distilled water, rinsing with alcohol to remove water, and a final rinse with ether to remove the alcohol . b. The pycnometer is filled with distilled water to the cali- bration mark, and the weight of the pycnometer and water is recorded (W ). The temperature of the water is recorded to the nearest 0.1 C (T.). Extreme care must be exercised to ensure that the water is well mixed and that the recorded temperature represents the true temperature of the water. The height of the thermometer bulb within the water should be noted so that the bulb may be held at the same level for subsequent readings . c. The weight of the pycnometer plus distilled water for any temperature (T ) can be caluclated from the formula x 18 density of water at T p W (T ) = ; zr I (W (T. ) - W.) + W. I (1) a v xy density of water at T. Lv av 1 ' V fJ v ' 1 d. Densities for various temperatures may be inserted in this formula to obtain values for the calibration curve. Figure 1 is an example of a calibration curve for a 100 milliliter pycnometer. 3 . Sample Preparation The sediment sample may be either at its natural water content or oven-dried, and slightly different procedures are prescribed for each case. Only the oven-dried sample procedure will be outlined here. The material is dried for at least 12 hours, or to constant weight, in o o an oven maintained at 105 C + 5 C. The sediment particles contain a film of absorbed water which must be removed, and the specific gravity obtained is dependent to some extent on the method of drying employed [ Lambe , 1949]. Careful control of the drying is required for all samples of the same material for consistent results. Upon completion of the drying period the samples are cooled to room temperature in a des iccator . 4. Specific Gravity Determination Procedure a. An oven-dried sample of at least 25 grams is added to a 100 milliliter volumetric flask, and the sample dry weight, W , is recorded to the nearest 0.01 grams. b. Distilled water is added to the flask, and the sample is allowed to soak for 12 hours. c. Additional distilled water is added to fill the flask about three-fourths full. d. The entrapped air is removed by i) gently boiling for ten minutes while continually agitating the sample, or ii) applying a 19 t UJ -I I- o o = o h CM % CM iO CM 8 S ii E -|8 ID CM 3 O o UJ I UJ 0. UJ o IO o o 01 > u 3 u c o •H ■u CO l-i CO O o s 8 8 8 a 8 8 8 swvd9 'aaivM aamisia aw 3~iiiog jo 1H0I3M IT) o >-l 3 M 20 vacuum, not exceeding 100 millimeters of mercury, to the flask. For oven-dry samples approximately two to four hours of vacuum application are usually necessary. e. If the sample is boiled to assist in removal of air, it is allowed to stand, preferably overnight, to cool to room temperature. f. The flask is then filled with distilled water until the bottom of the meniscus is even with the calibration line on the neck of the flask. g. The outside of the flask is cleaned and any moisture adhering to the inside of the bottle neck above the calibration line is removed . h. The flask and contents are weighed to the nearest 0.01 gram, and the weight recorded as W, . i. The temperature, T , of the suspension to the nearest 0.1 C is obtained. j. The weight of the bottle filled to the calibration line with distilled water only, W , is determined from the calibration curve for a the particular flask in use. T is used as the entry parameter for the X curve . k. The specific gravity of the sample, based on water at temperature T , is calculated using: ,T W r (_£) m 2 (2) sVr; w + (w - w, ) K } x o a b The results of equation (2) are multiplied by the relative density of distilled water at temperature T to obtain the specific X gravity relative to distilled water at 4 C. Equation (2) then becomes 21 ,Tx Wq Dx Gs '<7Zy = W + (W - W, ) (3) 4 C o a b where D is the relative density of distilled water at T . Tables of x x the relative density of water for various temperatures are available in handbooks . 5 . Discussion of the Bottle Pycnometer Method The primary advantage of this method is its acceptance as the standard procedure for the specific gravity determination of both terrestrial and marine soil particles. The great majority of specific gravity determinations have been made by this method. The technique is highly repeatable for the same material if sufficient care is paid to the drying method, weighing technique, visual estimate of the bottom of the meniscus at the calibration mark, and procedure for air removal. It is generally recognized that incomplete air removal from the suspended matter is the most common error associated with this procedure. If excess air bubbles remain in the suspension, the com- puted specific gravity value will be lower than the true value. In order to determine if the sample is sufficiently de-aired, the valve on the vacuum line to the flask is closed, and the stopper on the flask is slowly removed while observing the water level in the neck of the flask. If the water surface is lowered less than one-eighth inch for a standard 500 milliliter volumetric flask, the sample is considered qual e I y de-aired . The specific gravity computation equation involves a difference in weights which i . .:n,i J] in comparison to the weights themselves; irate v/. 1,'h! v ■ .i lii. .in produce errors in specific gravity 22 results. Sources of improper weights stem from (1) imprecise weighing of flask, water, and sample; (2) unclean flasks; (3) moisture on the outside of the flask or on the inside of the neck; and (4) improper visual setting of the meniscus at calibration line. If the material is boiled while vacuum is applied, some of the sample may possible be lost if the procedure is not closely monitored. If the temperature of the flask and contents is not uniform, an unrepresentative temperature may be obtained which would affect the results. The biggest disadvantage of this method is the time required to complete the analysis. After the sample is dried for twelve hours an additional twelve hours of soaking in distilled water is required prior to air removal. If the boiling technique is utilized for air remove 1, an overnight cooling period is necessary prior to weighing the flask and contents. Soil mechanics procedures usually recommend two to four hours as a minimum for de-airing by evacuation. Some investi- gators have found that additional evacuation in excess of 24 hours is necessary for accurate results. These requirements turn the specific gravity determination into a three day procedure. Air Comparison Pycnometer The Beckman Model 930 Air Comparison Pycnometer [Beckman Instru- ments, Inc., 1965] is a manually-operated device designed to measure the volume of powdery, granular, porous and irregularly-shaped solids. The instrument measures the true volume of the solid portion of a sample and excludes pore openings. Volume determinations of particu- late matter up to 50 cubic centimeters can usually be made by an experienced operation with repeatability of better than + 0.05 cubic 23 centimeters. The weight of the sample can be obtained by standard methods to provide the other value necessary for the specific gravity determinat ion . 1 . Principle of Operation Figure 2 is a schematic drawing of the Beckman Air Comparison Pycnometer. The instrument basically consists of two cylinders and two pistons with interconnecting piping, valves, and a differential pressure indicator. The reference cylinder contains two positive stops for the reference piston. A digital counter to indicate the sample volume is connected to the measuring piston. The measuring cylinder is connected to the sample container. When the coupling valve is closed and the sample cup locked in place, the differential pressure indicator indicates the difference in pressure between the measuring and reference cylinders. In this con- dition, and with no sample in the cup, any movement of one piston must be accompanied by a movement of identical stroke on the other piston to maintain a null reading on the differential pressure indicator. If both pistons are positioned in the forward position and advanced simultane- ously until the reference piston is against the rear stop, the counter should indicate zero volume. If this procedure were repeated with a sample of some volume, V , in the cup, and the pistons advanced the same distance, the pressures in the two cylinders would not be the same. A null pressure differential could be obtained by withdrawing the measuring piston some distance, d . This distance, d , is related x x the volume, V , and is calibrated so as to read the volume directly in cubic centimeters on the counter. 24 — i Eujk Egg o o x u -i 0) c u § OB -r-l H s. § ■H < O 4) w u T-t 27 o cu 8 ! S 8 2 5 28 29 3 . Operating Procedures The following three procedures were used in a comparison test to be discussed later. The helium (1-1/2-1 atmospheres) pro- cedure is a combination of two of the basic operating modes. a. Air Procedure (1-2 atmospheres) (1) Initially a zero measurement check is conducted. The procedure is identical to the measurement procedure, but a clean and empty sample cup is used. If the result of this check is other than zero, a second zero measurement check is made to verify the zero off-set. Once a zero off-set value is established, it is used as a tare number to correct subsequent volume determinations. A tare number greater than zero is subtracted from subsequent determinations, and a tare number less than zero is added. (2) The purge valve is closed, and the coupling valve is opened . (3) The piston handwheels are rotated to their counter- clockwise extreme positions. (4) The measuring handwheel is turned clockwise until the starting number is set on the counter. This is a calibrated starting position for the measuring piston that allows full stroke on the measuring piston to equal full stroke on the reference piston . (5) The sample is placed in the cup and the cup firmly locked in the sample cup compartment. (6) After a 15 second wait to equalize pressures between the two cylinders the coupling valve is closed. 30 (7) Both handwheels are simultaneously turned clockwise until the reference handwheel rests against its stop. The differ- ential pressure indicator is kept on the scale during this process. (8) After a 10 second wait the pointer on the differ- ential pressure indicator is brought to the null position by turning the measuring handwheel only. (9) The coupling valve is opened while noting the position of the differential pressure pointer. If the pointer does not shift as the valve is opened, a true null was obtained and the sample volume is read directly from the digital counter. If the pointer shifts, the run should be repeated. (10) Both handwheels are turned counterclockwise to rest against the stops. This step is essential to reduce the system pressure from two atmospheres to one atmosphere. If the cup were released prior to this step, the sample would be blown out of the cup due to the excess pressure in the system. (11) The sample cup is removed, and the pycnometer is now ready for another determination starting with step (3). b. Helium Purge Procedure (1-2 atmospheres) (1) The three-valve manifold is mounted on the air com- parison pycnometer as shown in Figure 3. The manifold gas valve is connected to the helium tank regulator and the vacuum valve to the vacuum pump. The helium regulator is set for 2 psig inlet pressure . (2) A zero measurement check is made to establish a tare number. This check is run using the helium purge procedure instead of the air procedure. 31 (3) The measuring and reference piston handwheels are rotated to their counterclockwise extreme position- (4) The measuring handwheel is turned clockwise until the starting number is set on the counter. (5) The sample is placed in the cup and the cup is locked firmly in its compartment. (6) The purge valve and then the coupling valve are opened . (7) The manifold vacuum valve is opened and the system is evacuated to the desired pressure. After evacuation is completed, the vacuum valve is closed. (8) The gas valve is opened for at least 5 seconds to allow the helium to purge the system. The gas valve is then closed. (9) The vent value is opened for 5 seconds to vent the system to the atmosphere. The vent valve and then the purge valve are closed. (10) The coupling valve is closed after waiting 15 seconds for pressure equilibration between the two cylinders. (11) Both handwheels are turned clockwise simultaneously until the reference piston rests against its stop. The differential pressure pointer is kept on its scale during this process. (12) After at least a 10 second wait, the pointer is brought to the null position by turning the measuring handwheel only. (13) The coupling valve is opened while observing the differential pressure pointer. If the pointer shifts position, a true null was not obtained and the run should be repeated. If the 32 pointer did not shift, the sample volume is read on the counter directly in cubic centimeters. (14) Both handwheels are turned counterclockwise to rest against their stops. (15) The sample cup is removed and a new volume deter- mination may be started with step (4). c. Helium Purge Procedure (1-1/2-1 atmospheres) (1) The three-valve manifold is mounted on the air com- parison pycnometer, the gas valve is connected to the helium tank regulator, and the vacuum valve is connected to the vacuum pump. The helium regulator is set for 2 psig inlet pressure. (2) A zero measurement check is conducted to establish a tare number . (3) The reference handwheel is rotated clockwise to its forward stop. (4) The measuring handwheel is turned to the estimated sample volume . (5) The sample is placed in the cup and the cup is firmly locked in place . (6) The purge valve and then the coupling valve are opened . (7) The vacuum valve is opened to allow the system to evacuate and the valve is closed after approximately 15 seconds. (8) The gas valve is opened for about five seconds to allow the helium gas to fill the system and then the valve is closed . 33 (9) The vent valve is opened for about five seconds to vent excess pressure to atmosphere. The vent valve and then the purge valve are closed. (10) The reference handwheel is rotated counterclockwise to its rear stop. The measuring handwheel is rotated counterclock- wise to a point beyond the starting number and then clockwise to the starting number. The system pressure is now approximately one-half atmospheric pressure. (11) After a ten second wait for pressure equilibration between the two pistons, the coupling valve is closed. (12) Both handwheels are turned simultaneously until reference handwheel rests against its stop. The differential pres- sure pointer is kept on scale during this process. System pressure is again at one atmosphere. (13) After a 10 second wait, the pointer is brought to the null position using the measuring handwheel only. (14) The coupling valve is opened while checking for a shift of the differential pressure pointer. If the pointer remains steady, a true null was obtained and the volume can be read on the digital counter . (15) The sample cup is removed and another determination is commenced at step (4). 4 . Discussion of Gas Pycnometer Method The primary advantage of the air comparison pycnometer is the Ldity of the volume determinat Lon. A maximum time of five minutes is required per determination regardless of the procedure used. The 34 sediment sample is usually oven dried for twelve hours at 105°C + 5°C and then ground in a mortar and pestle to a fine powder. The device is simple to operate and only requires that the operator familiarize himself with its characteristics to gain a feel for when the ref- erence piston is against the stop in either direction. The equipment is portable and could be used at sea. If the problem of weighing while aboard a ship at sea is solved, the pycnometer could be readily utilized in a sea-going laboratory to determine specific gravities. The air comparison pycnometer is somewhat temperature sensi- tive, and should be in approximate temperature equilibrium with its surroundings. Both the sample and sample cup should be within 5°F of instrument temperature. This requires the cooling of the sample to room temperature after the drying procedure. The two most common sources of error in volume determinations are failure to firmly lock the sample cup in place and excessive temperature differential between the sample and the system. Both sources of error are evidenced by a drifting differential pointer at the end of the run. Extreme cases are easy to distinguish, but a slight leak or small temperature differential is difficult to distinguish from needle drift due to surface activity of the sample. Jolly Balance The Kraus Jolly Balance, shown by Figure 6, is a hydrostatic weighing instrument requiring only two readings and a single division to compute specific gravity [Kraus, Hunt, and Ramsdell, 35 ur< 6 . Kim. fo Ily Ba lam e 36 1951]. One reading is made with the sample in air, and the second reading is made with the sample immersed in water. The balance con- sists of a single spring attached to a movable tube, which also carries a doubly graduated scale. The left-hand and right-hand scales are read using their verniers. In the determination pro- cedure the left-hand scale indicates movement of the scale to com- pensate for spring elongation due to the sample being placed on the upper pan. The right-hand scale indicates scale movement to compen- sate for spring contraction when the sample is immersed in the fluid on the lower pan. Two springs, light and heavy, are utilized with the instrument. 1 . Determining Proper Spring to Employ The sample weight is determined to the nearest gram. The light spring is used as supplied for samples weighing between one and ten grams. For a sample weighing between ten and twenty grams, cut off a portion of the spring until a maximum elongation of 40 centimeters is reached with a load of 22 grams. The heavy spring is used as supplied with a sample weight between twenty and fifty grams. For a sample weighing between 50 and 100 grams, trim the length of the spring until a maximum elongation of 40 centimeters occurs with a load of approximately 100 grams. Basically the determination should be performed with the spring near the point of maximum elongation for greatest accuracy and repro- ducibility of results. 37 2 . Sample Preparation The sample is first oven dried at 105 C + 5 C for twelve hours, and then allowed to cool to room temperature in a desiccator. Sediment samples should be ground to a fine powder in order to remove impermeable void spaces. 3 . Specific Gravity Determination Procedure Initially the two verniers and double scale are adjusted to a zero reading at the top of the instrument. A beaker of suitable size, usually 100 to 250 milliliters, and filled with distilled water is placed on the support shelf. The appropriate spring is suspended from the over-hanging support arm with the index rod and reading disk, metal pan, and glass pan attached in that order. The glass pan is immersed in the water by adjusting the beaker support shelf until the metal pan is one to two inches above the water level. Further zeroing is accomplished at this point to ensure the index disk is lined up with the horizontal mark on the mirror. Coarse adjustment is accomplished by raising or lowering the mirror support on its support rod. Fine adjustment is made by manipulation of the adjusting screw on top of the mirror. The instrument is now ready for a specific gravity determination using the following procedure. a. The sample is placed on the upper metal pan. By means of the large handwheel on the left hand side of the instrument, the scale is moved up until the index disk is in line with the mirror, indicated in Figure 6. 38 b. The weight of the sample in air is obtained by reading the left-hand scale from the top down, employing the fixed vernier. c The scale is then clamped by means of the knurled knob on the lower right-hand side of the instrument. d. The sample is moved to the lower glass pan by lowering the beaker, transferring the sample, and raising the beaker until the metal upper pan is approximately 1-1/2 inches above the water level. It is important that no air bubbles remain attached to the sample or pan. e. The large handwheel is turned clockwise, thus lowering the scale until the index disk is coincident with the line on the mirror. f. The second reading required is now made on the right-hand scale using its vernier. The reading represents the loss of sample weight when immersed in the water. g. The specific gravity is calculated by dividing the weight in air determined in step b. by the loss of weight from step f. 4- Discussion of Jolly Balance Method Specific gravity determination by this method is quick and easy. Other fluids more compatible than water with the material to be tested may be used. This instrument was compared with the Beckman Air Com- parison Pycnometer by Mclntyre, Welday, and Baird [1965]. The material used for the evaluation was granite rock. In that study specific gravities of 30 coherent rock specimens were determined in duplicate by both air pycnometer and Jolly balance, and a statistical analysis was performed on the results. Standard deviations were 0.0057 and 0.011 for the Jolly balance and air pycnometer, respectively. In that samples of only six to ten cubic centimeters were used, the evaluation was biased in favor of the Jolly balance. The full length of the Jolly 39 scale was used, while the air pycnometer, with a sample cup capacity of 50 cubic centimeters, operated at less than one-quarter of its theoreti- cal capacity. Further evaluation of the air pycnometer was conducted utilizing larger sample sizes, and it was concluded that the air pycnometer was superior to the Jolly balance if larger sample sizes were utilized in the air comparison pycnometer. The Jolly balance is primarily used by geologists and mineralo- gists to determine the specific gravities of fragments and chips of minerals or coherent rocks. The procedure does not appear compatible with the analysis of fine particulate matter as no provision is made for the removal of air from the sample when immersed in the fluid. Berman Density Balance The Berman Density Balance shown in Figure 7 consists of a sensitive torsion balance equipped with special accessories for the rapid measurement of specific gravity. The instrument uses the hydro- static weighing principle and can be read to the nearest 0.01 milligram. The range of the balance is zero to 25 milligrams with no counterweight n the counter-weight arm. The addition of a 25 milligram weight on the counter-weight arm will result in a range of 25 to 50 milligrams. A maximum weight of 75 milligrams may be attained with the use of counter- wc i ghts . A weight determination is made by suspending the sample from the I'll ii • arm. Two device; for holding samples are also shown in Figure 7. Th( d ill) lc weighing pan is made of very fine platinum wire and has • in upper plal form pan for weighing (he sample in air. Below the pan is 40 VERNIER BALANCE POINTER COUNTERWT, ARM ZERO ADJUST. KNOB DOUBLE WEIGHING PAN BALANCE ARM PEDESTAL PEDESTAL ELEVATION KNOB BALANCE RELEASE WIRE HOOK AND BASKET Figure 7. Berman Density Balance 41 a coiled helix to hold the sample for immersed readings. For weighing many small mineral fragments the wire hook and basket is used. The basket is made of 220-mesh screening and is hung on the lower or upper hook for weighings in or out of the fluid, respectively. The liquid is held in a small glass beaker on the pedestal and may be elevated or lowered by the pedestal elevation knob. Water, toulene, or any other fluid suitable for the sample being weighed is used. Toulene is preferred over water because of its lower surface tension. 1 . Sample Selection and Preparation The optimum sample weight to be used with the Berman Balance is between 15 and 25 milligrams. The accuracy of measurement decreases rapidly for samples weighing less than 10 milligrams. Samples over 25 milligrams require the addition of a counterweight to extend the range of the instrument. Larger sample weights also result in a loss of accuracy, especially those in excess of 50 milligrams. Particular care must be exercised in selecting the sample. Single grains should be used if possible. Coarse powders can be mea- sured using the fine mesh basket. If possible, the sample should be washed in the immersion fluid prior to testing. 2 . Balance Preparation An initial zero adjustment must be made with the sample holder suspended from the balance arm and immersed about half-way in the fluid. The balance arm is released by turning the balance release to its horizontal position. The index lever is adjusted until the zero on ernier coincides exactly with the zero on the dial. The balance ter, which is attached to the balance arm, should coincide with its ' line. If it does not , the zero adjust knob is used to bring the 42 pointer to zero. The balance pointer swings in front of a small mirror, and for a perfect zero adjustment the pointer, its image in the mirror, and the zero line must all coincide exactly. When this alignment is accomplished, the beam is in balance and ready for use. 3 . Specific Gravity Determination While the balance release lever is in the locked position, the sample is placed on the upper pan by allowing it to slide from a V-shaped piece of paper. The balance arrest mechanism is then released slowly to ensure that the hanger does not dip abruptly into the liquid. When the balance is fully released the sample weight is determined in air. At this time the lower pan is immersed in the liquid. For con- sistent results it is useful to bring the lower pan to the same depth in the liquid for every reading. This cancels surface tension effects and the weight of the immersed wire. To transfer the sample to the lower pan, the balance is arrested and the sample hanger removed from the hook with tweezers. The level of the liquid should not be changed. Using a needle or other small implement the sample is moved from the top pan onto a piece of paper and then allowed to slide into the lower basket. The hanger should be held vertically with the lower container just touching the surface of the table for support. The hanger is replaced on the balance arm hook, the balance is released, and the sample weight in the liquid is read on the vernier. Specific gravity is then calculated by dividing the weight of the sample in air by the loss of sample weight in the fluid with correction factors applied for the density of fluid used and the fluid temperature. 43 4. Discussion of Berman Density Balance Method The Berman Density Balance technique is simple and rapid. A specific gravity determination may be conducted in five minutes. Berman [1939] reported the obtainable accuracy is 0.2 percent with a 25 milligram specimen of specific gravity of 5. Using a large number of fragments of total weight of 25 milligrams, specific gravity five, and weighing in a basket, the accuracy is reduced to one percent. The instrument is not considered adequate for specific gravity determinations on marine sediments because of (1) the small sample size, and (2) the lack of provision for de-airing the sample. A three inch interval of a core sample two inches in diameter weighs well in excess of 100 grams. A 25 milligram specimen of this core sample would, in all probability, not be representative of the specific gravity of the core interval. A sample of fine particulate matter might fall through a wire mesh basket when immersed in the fluid. A solid container would allow the entrapment of air in the sample as the container is immersed. Either occurrence for the small sample weight used with this instrument would give an erroneous reading for fine particulate samples. Differential Gravity Tube A differential gravity tube is a mixture of two fluids in a column whose specific gravity varies from top to bottom. The fluids are com- monly known as heavy liquids. Heavy liquids have been used for many years as a means of mineral separation or ore dressing. Their use for gravity determination is an application of the flotation •I. The initial employment of this method consisted of adding an 44 unknown sample to a liquid of known specific gravity. According to whether the sample sank or floated the solution was either diluted or concentrated by adding another liquid until the sample assumed a position of hydrostatic equilibrium in the mixture. At that time the specific gravity of the sample is the same as that of the fluid and the specific gravity of the fluid mixture was determined by other means. Centrifugation was used to accelerate this process. (See Shapiro [1969] for an application using centrifugation.) The specific gravity gradient column has developed from the original use of the sink or float test. 1 . Preparation of Tube for Use A differential gravity tube is formed by the incomplete mixing of two miscible heavy liquids of different specific gravities in a graduated cylinder or burette. The choice of heavy liquids for use in the tube varies according to the range of specific gravities expected in the materials to be tested. Some typical heavy liquids are acetylene tetrabromide , bromobenzene , methylene iodide, and thallium malonate- formate . The best method for mixing the heavy liquids, according to Canada and Laing [1967] is to introduce the heavier liquid at a con- stant flow rate into a mixing chamber containing the lighter liquid and letting the mixture of increasing specific gravity flow into the gradient tube. The gradient will be linear if the flow rate into the gradient tube is twice the flow rate of the heavier liquid into the mixing chamber. Small calibration floats are used to establish the character- istics of the gradient. These reference floats may be obtained with a specific gravity accurate to four decimal places. The reference 45 floats are added to the column, and when they reach hydrostatic equilibrium their position is precisely measured. A calibration curve is prepared plotting specific gravity versus depth in column by means of the reference floats. 2 . Specific Gravity Determination The sample material is added to the column and when it reaches its equilibrium position, its depth in the column is precisely mea- sured. The intersection of this depth with the reference standard calibration curve then indicates its specific gravity. 3 . Discussion of the Differential Gravity Tube Method The stability of the specific gravity gradient established in the column is dependent on the diffusion rate of the heavy liquids used, frequency of use, and the agitation of the column created by adding samples or clearing the column. With proper care and tempera- ture control the column may be expected to maintain a closely linear gradient in excess of two months. This particular method is simple to apply, and the time required for a determination depends primarily on how fast the sample reaches its equilibrium position. Accuracy depends on the range of the specific gravity differential in the column, the age of the column, and the means used to measure the position of the samples in the column. The method is applicable to the specific gravity determination of individual small particles. Sediments and soils are aggregates of minerals having a variety of specific gravities. The constituents of a sample of fine-grained, powdered, marine sediment would spread throughout the column, with each constituent seeking its equilibrium 46 position. The required weighted average of the specific gravities of the particular mineral assemblege in the sample is not directly provided by this method. It is also recognized that a small specimen is not representative of the specific gravity of considerably larger samples. For these reasons, the flotation method, in general, is not suitable for the specific gravity determination of marine sediments. Derived Equation for Specific Gravity Computation From the basic definitions for water content and bulk wet density equation (4) was derived for the computation of specific gravity . G = 525 s 1 + WC - (BWD X WC) ' v ' G = specific gravity of solids, WC = water content (percentage), BWD = bulk weight density (grams per cubic centimeter). It was assumed for the derivation that the water evaporated from the sample during the water content determination is salt-free with a specific gravity of one. A correction for dissolved solids from the sea water remaining in the sample after evaporation was considered to be negligible for the purpose of applying this equation. The complete derivation of equation (4) is shown in Appendix C. Two sets of data containing values of water content, bulk wet density, and specific gravity were obtained to determine the validity of equation (4) as a means of obtaining an accurate value of specific gravity of solids. The first set was secured from the Naval Civil Engineering Laboratory, Port Hueneme , California, and pertains to 42 cores collected from the Eastern Pacific Ocean and analyzed during 47 1963 and 1964. Water content was determined by obtaining a quantity of the sample in a cylinder of known weight and determining the weight of the wet sample. The dry weight was determined after the sample was oven dried over night at 100 C and cooled in a desiccator. Water content was then computed by dividing the weight of the water by the weight of the solids. Bulk wet density was determined by using a small cylinder of known volume and determining the weight of the undisturbed wet sample necessary to fill it. The bulk wet density was then computed by dividing the wet sample weight by its volume. The specific gravities for this same material were determined with a Beckman Air Comparison Pycnometer using helium as the comparison medium. A computer program was written to calculate the specific gravity using equation (4) and to compare these computed values with those determined by the air comparison pycnometer. A difference representing the gas pycnometer value minus the calculated was computed and recorded. The computer program is contained in Appendix D. Fifty-six percent of the computed specific gravities were greater than the air comparison pycnometer values for the 386 intervals from these cores. In general it may be noted that the comparison was very poor, with only 10 percent of the computed values agreeing to within + 0.05 of the pycnometer values. The computer output for the Naval Civil Engineering Laboratory data is included in Appendix E. A second set of data, obtained from Technical Report Number 106 of the U. S. Naval Hydrographic Office by Richards [1962], was treated in a similar manner. The water content and bulk wet density were determined using essentially the same techniques as were used for the 48 NCEL data. Specific gravities weie measured by the bottle pycnometer method using 100 milliliter flasks. Some 180 intervals of sixteen cores from this data were subjected to the computer program. Thirty- two percent of the specific gravities computed by (4) were greater than the bottle pycnometer values. Forty-five percent of the calculated specific gravities agreed within + 0.05 of the bottle pycnometer values. The computer output for the Hydrographic Office data is included in Appendix F. Equation (4) was derived to make possible the use of water content and bulk wet density values, which are routinely determined during the physical processing, to calculate specific gravity easily. This would thereby eliminate the need for the questionable and time- consuming specific gravity determination. The results of this investigation of the two sets of data indicate that accurate specific gravities, as compared to actual determinations by either bottle pycnometer or gas pycnometer, are not attainable by equation (4). The probable causes for the inadequacies of this calculation are inaccuracies in the techniques for the determination of water content and bulk wet density. 49 IV. COMPARISON OF AIR COMPARISON PYCNOMETER AND BOTTLE PYCNOMETER METHODS General The general acceptance of the bottle pyncometer as a standard method for specific gravity determination for sediments has been cited previously along with the advantages and disadvantages of the procedure. The time reduction per specific gravity determination offered by the gas pycnometer warranted an evaluation of the device in comparison with the bottle pycnometer. There have been numerous articles published that evaluate the characteristics of the gas pycnometer (Beckman Instru- ments, Inc. [1960], Joyce [1961], Meinhall and Buckingham [1962], Landy and McGahan [1963], Price [1964], Mitchell [1964] and Tuul and DeBaun [1962]). However, the majority of these have used air as the comparison medium with only two using helium in their tests. For the above reason, three operating modes of the gas pycnometer, two of which use helium, were compared with results of the bottle pycnometer method. The gas pycnometer modes tested were the air (1-2 atmospheres) procedure, the helium (1-2 atmospheres) procedure, and the helium (1-1/2-1 atmosheres) procedure. Inclusion of the helium its was considered necessary in view of the need for a means of accural' Lume determination of colloidal materials. Figure 8 is ' ture I the laboratory equipment used for the bottle pycnometer its. Figure 9 shows the air comparison pvcnometer with the vacuum pump and helium tank attached to the helium purge manifold via plastic ( lib i Figure 8. Equipment Used for Bottle Pycnometer Determinations Figure 9. Air Comparison Pycnometer with Vacuum Pump, Helium Bottle and Regulator 51 A similarity between the earlier gas pycnometer evaluations noted above was their common use of a comparison technique in which a specific gravity value measured by one technique was compared with another value for the same sample found by a second technique. Such testing on a one for one comparison basis does not provide sufficient repetition to reveal an error in either of the techniques for any one test material under observation. In addition it does not permit the establishment of a mean value and variation for the compared techniques, whereby the accuracy and precision of the methods may be established. Statistical analysis using analysis of variance techniques as discussed in Ostle [1963], provides a sound basis for comparing two or more methods and hence was chosen to compare the bottle and gas pycnometers . The BIMED Analysis of Variance for One-Way Design was used as the statistical analysis tool. This computer program is the version of June 15, 1966, developed by the Health Services Computing Facility at the University of California at Los Angeles [Dixon, 1968]. The statis- tical analysis procedure required the determination of a specific gravity value using each of the three gas pycnometer modes and also the bottle pycnometer method for a number of samples of each test material. The number of samples of each test material required was chosen to obtain an adequate number of degrees of freedom to ensure a low critical F-ratio. A low critical F-ratio ensures less chance of rejecting the null hypothesis for the experiment if the null hypo- thesis is actually true. The null hypothesis applied to each test material was that there is no significant statistical difference between the specific gravity values determined by the three gas pycnometer modes and the bottle pycnometer method. 52 It was desired to obtain test materials with an established specific gravity that exhibited the colloidal properties of marine sediments. A quantity of material with consistent constituents was required such that replicate determinations could be made on a number of samples for statistical analysis purposes. The analysis of variance technique requires the assumption that the samples chosen from a quantity of test material be consistent. The selection and preparation of the sample material was designed to meet this requirement Suitable test material, having specific gravity values known to three decimal places, was not readily available. As a consequence, quantities of the American Petroleum Institute reference clay samples were procured for test purposes. Kaolinite (A. P. I. reference clay #4) and montmorillonite (A. P. I. reference clay #25) were selected because of their reported purity and differing physical and chemical characteristics. These clay minerals are two of a group of selected clay samples collected at the same localities in the United States from which the original reference clay samples were obtained that served as the basis for American Petroleum Institute Clay Mineral Standards Project No. 49. The identity of these clays with original A.P.I, clay mineral standard specimens had been previously established for the commercial source by direct comparison of X-ray diffraction and differential thermal analysis data on the new material and the original standards . In that the true specific gravities of the kaolinite and mont- morillonite clay samples were unknown except for reported values of comparable materials found in other literature, crystalline quartz was used as an established reference standard. The specific gravity 53 values of quartz at various temperatures has been summarized by Fronde 1 [1962]. Tests were run on the quartz material in the same manner as for the reference clay samples and the results were statistically analyzed . An additional comparison of the gas pycnometer and bottle pycno- meter was made using alternate four inch intervals of a fifty inch sediment core. Although statistical analysis is not applicable to these results, individual comparisons for the eight intervals tested c ou Id be made . Sample Preparation The sample materials were prepared for testing with a consideration for the requirements of both the gas pycnometer and bottle pycnometer procedures and the need for homogeneous samples for valid statistical analysis. The kaolinite was received in the form of large dry lumps. Approximately 500 grams were hand-ground in a ceramic mortar and pestle to a very fine powder, and then divided into ten samples of 50 grams each, which were oven dried at 105 C + 5 C for twelve hours. The samples were then placed in a desiccator and cooled to room tempera- ture prior to testing. The montmor i 1 lonite contained some of its natural moisture and ice was oven dried for six hours prior to grinding. Approximately 500 grams of the pre-dried material were then ground, divided, oven- dried, and cooled in a desiccator in the same manner as the kaolinite. The quartz was received in the form of crystals measuring approxi- ii. b me by two Inches. An attempt was made to use only the pure i Lps I the large cyrstals by crushing them into smaller 54 pieces and selecting the desired fragments. These fragments were then crushed into small chips using the cup and piston shown in Figures 10 and 11, and then placed in a ball mill for reduction to a coarse powder. Final grinding was done in either an automatic or manual mortar and pestle. After each phase of crushing or grinding, a magnet was used to remove metal fragments introduced by the crushing process. The powder was then sieved and 540 grams of quartz powder were collected that had passed the #230 sieve. This quartz powder was then divided into 12 samples of 45 grams each, oven-dried, and cooled in the same manner as the reference clay samples. Because the sediment core contained its original water content, it was pre-dried 18 hours prior to being ground into a fine powder. Fifty grams of each of the eight intervals were then oven-dried and cooled as were the previous samples. Additional drying of the montmori llonite and sediment core materials after the pre-drying and grinding was considered necessary in order to reduce the possibility of biasing the gas pyenometer determinations. Fine-grained dry colloidal material tends to absorb moisture from the atmosphere. Numerous checks were made on the weight of kaolinite and montmorillonite after 10 to 15 minutes of exposure to the atmosphere. These checks indicated a weight increase of approxi- mately 0.01 grams for a 40 gram sample in every case. Exposure of the samples to the atmosphere for an extended time could alter the specific gravity values. As a consequence all samples were dried for 12 hours after being ground and prior to their analysis. 55 Figure 10. Quartz Crushing Apparatus Figure 11. Quartz Crusher Components 56 Specific Gravity Results for Kaolinite 1 ■ General Kaolinite is a clay mineral having the general formula A1203 • 2Si02 • 2H20 in which the Al to Si ratio can vary from 2:1 to 3:1. It is a two-layer clay thereby composed of a single sheet of silica tetrahedrons and a single sheet of alumina octahedrons combined so that the tips of the silica tetrahedrons and one of the layers of the octahedral sheet form a common plane. Kaolinite single crystals have a ratio of area 1 diameter to thickness of from 2:1 to 25:1. Widths of 0.05 to 2.11 microns and lengths of 0.07 to 3.51 microns are common [Kerr, et al. , 1951] . 2 . Results The results of the specific gravity determinations on the ten kaolinite fractions are shown in Table I. An observed F-ratio of 167.99 as computed by the BIMED analysis of variance program far exceeds the critical F-ratio of 4.38 at the C(= .01 level of significance. There is a significant statistical difference between the specific gravity values determined by the four test procedures. The BIMED computer output is contained in Appendix G under the problem code SGKAOL. The specific gravity values determined by the bottle pycnometer method were dropped from the analysis of variance computation and for a null hypothesis it was assumed that there was no significant statis- tical difference between the specific gravity values determined by the three operating modes of the gas pycnometer. The observed F-ratio computed under these circumstances was 24.42. The critical F-ratio was 5.49 and the null hypothesis was rejected at the OC = .01 level 57 CO < QJ 4J o CO 14-1 o co cu , — I a, e « to c a> 4-1 co c o •H 4-J CO c •r-l E rJ 0) 4J QJ -a > CO )-i 60 O 0) Cl, CO CO ■u rH CO QJ < p 1 2 2 h-l O < > M H W H C/} O m CN] CM LO r~- co 00 r- r^ on 1 — r~~ m 1— 1 1— i 1— i LO CNI 00 10 CNI CNI CNI CNI X> CO CN| CNI ON LO r— 1 00 CNI 1 — rH O ON lO CNI CNI CNI CNI ON r-l LO X> r— 1 ON LO CNI CNI CNI CNI CO O 00 1— 1 00 ON r-l O X) CNI CN| CNI CNI lO lO 00 00 X> 00 LO PQ O a W QJ J-l •-n qj en xl QJ D. /-N U CO W QJ O QJ XJ E Ij ati 0) w co X! O a, E '-{ co -u ' O CO CN| /-N E "■"«. ^ 4-1 CNI >— 1 QJ CO 1 ' J-1 t— 1 r-l CO CNI S >1 1 r, .-. V—' XI ■h E E 3 3 M T3 •> -H «H QJ CU 14 rH rH *J c •r-l QJ QJ QJ •H CO X! XI E E W W N_X O U c QJ M M M U 4J QJ QJ QJ >N QJ 4-1 4-1 4-1 CL 13 QJ QJ QJ E E E QJ a> O O O 1— 1 u d c C 4-j a) O U U 4J ? >^ >, >, 0 CL CL CL X) w a) C C C U •1-1 O O O QJ 4-1 yj W CO 4-J >H ,,_| .r-| -r-l -r-l > Jj M kl I- 1 cO cO cO CO ••-I )-i CL CL CL, rH 00 E E E -1 O O O T-l U 0 0 0 E •r-l U-J S-l r4 VJ O •r-1 • r-l -H -r-l O O - > Z80 O U. o 85 2.60 A— A Air Pycno meter (1-2) a — n Helium Pycnometer(l-2) o — o Helium Pycnometerd-l/2-i) x — X Bottle Pycnometer -x- 2.40 4 5 6 7 SAMPLE* NUMBER 8 K) Figure 12. Graph of Kaolinite Results 60 tin' standard deviation. Gruner [1937] summarizes the specific gravities (if various samples of kaolinite. The nineteen values he listed included other investigators, as well as his own bottle pycnometer and centrifuge determinations and theoretically calculated specific gravities. The values ranged from 2.51 to 2.604, and then fell between 2.580 and 2.600. Though none of the samples were reference standard #4 material, the results substantiate the bottle pycnometer values obtained in this study . Specific Gravity Results for Montmori llonite 1 . General The clay mineral montmori llonite has the general formula 5A120 • 2Mg0 • 24Si0 • 6H 0 (Na 0 , CaO) and has a three-layer, expanding lattice. It consists of units made up of two silica tetrahedral sheets with a central alumina octahedral sheet. The stacking of the silica-alumina-silica units results in a very weak bond, which permits a lattice expansion when water or other polar molecules enter between the unit layers. Montmori llonite single crystals exhibit a ratio of areal diameter to thickness of from 100:1 to 300:1. 2 . Results The results of the specific gravity determinations on the ten montmorillonite fractions are shown in Table II. The observed F-ratio for this test was 44.96 as computed by the BIMED program and the critical F-ratio was 4.38. There is a statistically significant difference at the oC = .01 level of significance between the specific gravities determined by the four test methods. The 61 QJ 4-) •r-l C O CO QJ .—I a E CO co C OJ 4J 14-1 O CO c o •r-l 4-1 CO c •r-l E u CD 4J 01 -o 4-1 ■r-l > CO U bO U •r-l UH •r-l CJ QJ a CO U-l o CO 4-1 r-l 3 CO m O CN 00 m 00 1 — CM v£> 00 m O o CN CN CM 00 r^- 00 r^ PQ CJ CO QJ Vj r~\ 0) IT, -C r— \ QJ CL CO U CO QJ > 1 r. „ rQ 1—1 E E 3 3 rJ -o « •H •r-l QJ -4 r-l r-l CJ 4-1 QJ 01 OJ >. 01 4J 4J 4-J a, T3 QJ QJ QJ E E E QJ CO o o o ■— 1 u a c c 4J cu a u CJ 4-1 ? >. >% >, o CL CL a, jd CO 0) a C 3 r-l •r-l o o 0 OJ 4-J CO CO CO 4-J •r-l •H •r-l •r4 •r-l > rJ r-l u i—l CO CO cd CO •r-l rJ a, cx CL, r-l M E E E t— 1 o c O •r-l u CJ CJ a E •r-l M-l U r-4 u o •r-l •r-l •H •r-l o u < < < m 0) O, /"> /~\ r*"> ^-s CO < rq u a 62 ><>c BIMED computer output for this test is contained in Appendix G under the problem code name SGKAOL. The analysis of variance was re-run on the gas pycnometer values without the bottle pycnometer values. The observed F-ratio for this case is 63.24 and the critical F-ratio is 5.49. Thus the null hypothesis that there is no statistically significant difference between the gas pycnometer values is rejected at the dC = .01 level of significance. The BIMED computer output for this calculation is included in Appendix G under the problem code name SGMACP. 3 . Discussion of Results Figure 13 graphically illustrates the results of the mont- morillonite specific gravity determinations. As may be seen, the bottle pycnometer values fall below those of the air comparison pycno- meter except for sample #9. The bottle pycnometer determinations were made five at a time using approximately 25 gram samples in 500 milli- liter pycnometer bottles. A conspicuous difference was noted between the first and the last five of the determinations, which may be explained by more complete air removal in the case of the last five tests. For the first five determinations the bottles were evacuated for eight hours with random agitation throughout this period. The last five runs were evacuated for ten to twelve hours and each bottle was hand agitated for at least 30 minutes during the last three hours of the evacuation period. It may be seen that the last five of the bottle pycnometer values compare well with the gas pycnometer values using the helium (1-2 atomspheres) mode. The air operating mode gas pycnometer values are comparatively high and the furthest removed from the bottle pycnometer results, as was 63 3.20 r Q ^ 3.00 (O b 8 o 2JB0 - D u It CO 2$0 A— A Air Pycnometer ( 1-2) d — □ Helium Pycnometer (1-2 ) o — o Helium Pycnometer( I- 1/2-1) x — x Bottle Pycnometer 2.40 SAMPLE NUMBER 8 Figure 13. Graph of Montmori 1 Loni tc Results 10 64 the case for the kaolinite tests. The helium (1-1/2-1 atmospheres) mode values are slightly higher than the helium (1-2 atmospheres) values. This last observation for the montmori llonite samples is in opposition to the finding for the same two modes with kaolinite. The standard deviations for the gas pycnometer determinations range from 0.0172 to 0.0211, indicating the precision for the three modes is about the same. This is different from the standard deviations for kaolinite, where the precision varied with the operating mode. The standard deviation for the bottle pycnometer readings is high as a result of the large difference between the first and last five values. Various values for the specific gravity of montmorillonite are found in literature. Grim [1953] concludes that the value may range from 2.2 to 2.7 with even higher values possible for materials of high iron content. All of the specific gravity values for this test were higher than any found in literature. Specific Gravity Results for Quartz 1. General Silica exists in a number of different crystalline forms with quartz being the most common. Frondel [1962] indicates the specific gravity of quartz at 760 millimeters of mercury at 18 to 20 C as approximately 2.6510 referred to distilled water at 4 C. 2 . Results The results of the specific gravity determinations on twelve powdered quartz samples are shown in Table III. An observed F-ratio of 1.22 was computed by the BIMED analysis of variance program. The critical F-ratio for this test was 2.82 at the oC = .05 level of significance. The null hypothesis was therefore accepted for the 65 PQ 3 m 3 cr U-l o 75 0) r- 1 E co to CU > i— I 0) 3 w C o •1-1 4-1 Cfl c: > 4J > CO l»i 00 o •M o 0) co co i— I 3 co M • • • • H OS W H o o o o W 00 SO m en CN CM CM CM CM CM CM CM CN PQ CM CM CM CM CJ CM I— 1 sD m m m p»- m so so sO so en 00 ON •vf >fr m m sO m sO so sO sO CM CM CM in m r^ -* sO sO so sO CM as o sO m - sO sO sO so sO CM o 00 en m m r^- m sO sO sO so CN sO 00 o > 1 •1 •> s_/ -o 1—1 | E 3 b T3 « •fl •r-l (JJ 0) U rH r-l 4J c •r-l 0) CD CU •r-l CO J= J3 E E S-r- *^ V-r O U c CU u rJ rJ U u 0) . 9) j_> 4J 4J CU T3 cu 0) CU E E E cu CD o o O r-l u c c C -U s >, >. o Q. Cl Q. J3 CO OJ c c C r. •r-l o o O CU 4J CO CO CO 4J •r-l •r-l •r-l •rH -rH > u M rJ r-l cfl CO (T3 CO -r-l U Q. CX Q..-I 60 E £ E ^ O o O -H O o o o E ■t-t U-l u rJ rJ O •r-l ■r-l •^1 ■rJ O o 8. < <: < ^ x~\ >— \ /~\ ^— N CO < PQ U Q 66 quartz test. There is no significant statistical difference between the specific gravities obtained by the four determination techniques. The BIMED computer output for this test is contained in Appendix D under the problem code SGQUTZ . 3 . Discussion of Results Figure 14 is a plot of the results of the quartz specific gravity determinations. Two obviously erroneous determinations are apparent for the bottle pycnometer method, and these contribute to the large standard deviation for this method as compared to the gas pycno- meter modes. The bottle pycnometer values were determined three-at-a- time using approximately 25 gram samples in 100 milliliter flasks. Air removal was facilitated by boiling for 10 minutes under vacuum with continuous agitation followed by continued evacuation for 8 to 10 hours with random agitation. The gas pycnometer values for the helium (1-1/2-1 atmospheres) mode are all higher than the rest of the values, although the standard deviation for this mode compares favorably with the variability of the other two modes. It is believed that the zero-measurement check for this mode is not dependable, and may result in an erroneous tare number. The helium (1-2 atmospheres) mode mean specific gravity is very close to the known specific gravity of quartz, and its standard deviation is also small. The closest mean value and the smallest standard deviation for the quartz samples were for the air (1-2 atmospheres) mode. Specific Gravity Results for Sediment Core 1 . General The sediment core analyzed was collected off the California coast on 5 February 1970 at latitude 36°36' North and longitude 123°56' West 67 2S00r g 2B00 Li. o A— A Air Pycnom«ter(l-2) a — a Helium Pycnomtttr(l-2) o — o Htlium Pycnometer(l-l/2-l) x — X Bottlt Pycnomtttr < cr o o £ 2.700 K 2 600 4 5 6 7 8 9 SAMPLE NUMBER 10 II 12 ire 14. Graph of Quartz Results 68 in a water depth of 4200 meters. The core was approximately 50 inches in length, and alternate four inch intervals of the core were subjected to testing. 2 . Results The results of the specific gravity determinations on the eight sample core intervals are shown in Table IV. A statistical analysis is not applicable to these results. 3 . Discussion of Results Figure 15 is a graph of the results of the sample core specific gravity determinations. It is apparent that the bottle pycnometer values are generally lower than the gas pycnometer values. The helium (1-2 atmospheres) mode values are, for all intervals, closest to the bottle pycnometer readings. The air (1-2 atmospheres) mode values were intermediate to the helium mode values for the first three intervals, but the remainder of the readings were considerably higher than the helium values. Perhaps an incorrect tare was applied to the last four deter- minations for the air mode. Both the bottle pycnometer and gas pycnometer methods indicate a discontinuity, or low specific gravity value, in the middle of the core. The three gas pycnometer modes indicated the low value at the 19-22 inch interval, while the bottle pycnometer method indicated a low specific gravity at the 25-28 inch interval. 69 > H CO c 1-1 QJ 4J -C 00 •H QJ U-l o c o •H 4J to c ■1-1 E 0) J-4 — 1 QJ a 4-1 E QJ to TJ en >, QJ 4-1 >-i ■H O > o to ^ x: 00 u c o ■ ^ — 1 M-l o ■r^ in O QJ to Q. tn U-l O U-J O [« — 1 en % j-i > ^-< u 3 QJ w 4-1 01 c Cd •H v£> v£) co 1 ON 00 00 r~- co <}• CN CN CN CN o co co CN CM I CO > a: O c_> CO o> L/O m CM io i — i ON o> , 1 l-» o> cn r^ 00 . — i o v£> CN i — i 00 r»» O 1 o 00 00 vD m CN CO CN C\J CN 00 00 ON 00 o> On i—i 00 CM CO pq CO 00 00 1—1 o CO C_> ON r-. O o> i-- CO I — CM CN 00 CO CN o CN o> ON o> ON vD o cn QJ •**\ ^ CO QJ 01 X! /— N Vj a C/5 0) en QJ xi O M Cl E 0) co 4J XI o CO ex £ Cfl 4J 1—1 o cn 1 •^ E CN !-J 4.) CN — QJ CO 1 i— | 4_l .— 1 I cfl CN ^ S £>-> 1 •* ^-^ XI i—l E E 3 3 U T3 « •H ■r-l QJ QJ 1-J i— 1 i — 1 4J c •r-4 QJ QJ QJ • H (0 fl x; E E N— ' *— ' *— ' o Vj c QJ J-l S-i >-i o 4-) QJ QJ QJ >. QJ 4-J 4J 4-1 Q. T3 QJ 0) QJ E E E QJ QJ o a O --I S-i c c C 4-1 QJ o u O -u 3 >, >> >, o Q. a Cu ^d Cfl 0) c c C l-i ■i-l o 0 O QJ 4-1 cn w cn 4J •H ■H •i-i •H >i-l > Vj u ^J 1-1 CO CO cfl (0 -i-l J-4 Q. r_ CI, i—l 00 E E E -i o 0 O T-l u u u o E ■rH U-l 1-1 M ^ o •H ■H •H •M O o < < <; m QJ Q. •— N ^-\ / — ^ y—\ cn . Oceanography graduate student, plastic vial of known volume plus weight determination for wet density of marsh muds, accuracy of + 5$, Department of Oceanography, precision glass tube for volume plus weight for density of sediments . Department of Civil Engineering, bottle pycnometer for soils, accuracy of + 0.01 Department of Civil Engineering, bottle pycnometer for soils, accuracy to fourth dec ima 1 place . Department of Civil Engineering, bottle pycnometer for soils and clays, accuracy of + 81 Institution Comment Kansas State Co lie ;ge University of Kentucky Department of Civil Engineering, pycnometer for soils and clays. bottle Long Island University Louisiana State Univers ity University of Maine University of Mary land Massachusetts Institute of Technology University of Massachusetts McGill University University of Miami Michigan State Univers ity University of Michigan University of Minnesota University of Missouri University of H imsh ire University of : rk University i ty rk Department of Civil Engineering, bottle pycnometer for clays, accuracy of + 0.005. Department of Civil Engineering, bottle pycnometer for soils and clays, accuracy of + 0.01. Department of Civil Engineering, bottle pycnometer for clays, accuracy of + 0.01. Department of Oceanography, air comparison pycnometer for sediments, accuracy of + 10^>. 82 Inst i t ut i on Comment Un i vers i t y of Department of Geology, Berman Balance for small Notre Dame mineral samples. Department of Civil Engineer- ing, bottle pyenometer for fine grain soils and clays, accuracy of + 0.01. Ohio State Department of Civil Engineering, bottle Un i vers ity pyenometer for soils, accuracy of + 0.5. Old Dominion Coi lege Oregon State Department of Civil Engineering, bottle Univers ity pyenometer for soils, accuracy of + 0.01. Pennsylvania Department of Civil Engineering, bottle State University pyenometer for clays, ASTM tolerance + 0.002. University of Pennsylvania University of Department of Civil Engineering, bottle Pit tsburg pyenometer for soils and clays Princeton University Purdue University Department of Civil Engineering, bottle pyenometer for marine sediments and clays, accuracy of + 0.04. Queen's University Rensselaer Poly- Department of Geology, bottle pyenometer for technic Institute soil sediments. Department of Civil Engineer- ing, bottle pyenometer for soils and clays, accuracy of 1 in 300. University of Rhode Island Rugters University San Diego State Department of Civil Engineering, bottle Col lege pyenometer for soils, accuracy of + 0.01 after evacuation for 24 to 48 hours on vibrating table. San Francisco State College 83 Inst itut ion C omme n t San Jose State Colic ge Department of Geology, bottle pycnometer for minerals, accuracy within 1$ . University of Southern California Southern Methodist Univers ity University of Southern Florida Stanford University Syracuse University Department pycnometer of Civil Engineering, bottle for soils, accuracy of + 0.1. Univers ity Tennessee of Department of Geology, centrif ugat ion in constant density gradient liquid for minerals, density accuracy to + 0.005 gm/cc . Univers ity Texas of Agricultura Mechanica 1 of Texas 1 and College Department pycnometer of Civil Engineering, bottle for soils, accuracy of + 0.02. Univers ity of Utah Department pycnometer of Civil Engineering, bottle for soils . Vanderbi It Univers ity Univers ity Vi rginia of Department pycnometer of Civil Engineering, bottle for soils, accuracy of + 0.01. Un i vers ity i i ngton of Un i vers ity is i n of Department comparison + 0.5$. of Civil Engineering, air pycnometer for soils, accuracy Un i vers ity Department of Geology, differential gravity tube for minerals, accuracy of + .001. 84 LABORATORIES AND INDIVIDUALS Laboratory or Individual Phi 1 lip P. Brown Soil Mechanics Consultant Naval Facilities Engineering Command Michae 1 Duke U . S. Geological Survey Dr. I. Robert Ehrlich Davidson Laboratory Dr. Richard W. Faas Professor of Geology Lafayette College Dr. Chester Francis Health Physics Division Oak Ridge National Laboratory Mr. W. H. Glezen Gulf Research and Development Company Dr. Thomas Gold Department of Astronomy Cornell University Dr. M. Grant Gross Marine Sciences Institute State University of New York Dr. J. J. Grossman Missiles and Space Systems Douglas Aircraft Dr. George Keller Atlantic Oceanographic Laboratory ESSA Comment Bottle pycnometer to determine specific gravity of fine particulate matter to better than + 5$. Various methods to determine in-situ density of submerged soil sample. Isopycnic zonal centrif ugat ion to determine density of clays to + 0.05 g/cc depending on purity of sample . Air comparison pycnometer with helium to determine specific gravity of shales to + 0.5$ (i.e., 2.70 + 0.01). Air comparison pycnometer to deter- mine specific gravity of marine sediments. Accuracy never properly eva luated . Bottle pycnometer to determine specific gravity of marine sediments to + .005 accuracy 85 Laboratory of Individual Comment L. B. Macurdy Mettler Balance Company Dr. James Rucker Sediment Laboratory Naval Oceanographic Office Dick Seiter Bechtel Corporation Leonard Shapiro U. S. Geological Survey D. R. Stephens Lawrence Radiation Laboratory Howard Sutter Baroid Division National Lead Company Director, Geology Section U. S. Bureau of Mines Di rector Marine Geology Division She 1 1 Research F) i i inics D i v i . i )ii iy Expi it Stat Hydrostatic weighing techniques. Accuracy varies with size of sample. Bottle pyenometer to determine specific gravity of marine sediments. Repeatability to 0.01 to 0.02 specific gravity va lue . Bottle pyenometer to determine specific gravity to + 0 . 2j> . Sink-float technique to determine powder density of rocks. Sample size is approximately 50 mg . Accuracy + 0.04 gm/cc . Fabricates sample into known geo- metry and weighs it. Accuracy of density determination is + 0.2%. LeChatelier flasks to determine specific gravity to less than 1.0$. The bottle pyenometer used with accuracy to three decimal places. Samples of fine particulate matter are tested in a 500 ml. flask with de-airing by vacuum. The flask is placed in a water bath shaker main- tained around 20°C. The flask is weighed on a balance readable to 0.1 gm . Air comparison pyenometer also used with helium purge with accuracy of +.015. Primarily interested in bulk density rather than grain density. Bottle pyenometer method used. Duplicate tests are conducted and considered valid if results agree within + 0.01 . 86 COMMERCIAL FIRMS Name of Firm Comment Wm . Ainsworth, Inc. American Instrument Co., Inc. Bailey Meter Company The Bissett -Berman Corporation Brinkman Instruments, Inc. R. P. Cargille Labs, Inc. Cintra International Company Cox Instrument Curtin Scientific Company Eberback Corporation Engineered Materials Enraf -Nonius , Inc. Federal Scientific Company Fisher Scientific Company The Foxboro Company Gardener Laboratory, Inc. Geoliquids Division National Biochem Company Manufactures a number of balances which may be modified for specific gravity determination. Manufactures Kraus Jolly Balance which measures specific gravity of solids - sample weights up to 300 grams may be used. Distributes specific gravity testing set. Can be used for specific gravity determination of single mineral. Uses heavy liquids which are toxic. Generally used for heavy mineral separation. Manufactures Berman density balance. Range of sample size 15 to 25 mg. Manufactures density gradient tube and calibrated liquids. 87 Name of Firm Comment Gilford Instruments Lab., Inc. Gow-Mac Instrument Company Hallikainen Instruments The Heusser Instrument Manufactures model SG-203 balance Company (Utah) specifically for specific gravirv determination. Weighs up to 12 gram sample in air and in desired fluid. Simple calculation is required for specific gravity. Reading range: 0.62 g/ml -1.85 gm/ml to a 0.001 precision . Heusser Instrument Company West Coast Division International Light, Inc. Kay-Ray , Inc . Kimble Products Lab Glass , Inc . David W. Mann Company Microsca le , Ltd . Nuc lear-Chicago Numec Instruments and Controls Corporation The Ohmart Corporation Manufactures Model 310 and 311 balances which can be modified to make specific gravity determinations Si Lentif ic , Inc . Princo Instruments, Inc. Pro : Ler -Smith Manufactures Berman density balance. I ument Corporation 88 Name of Firm Comment Sclioeffel Instrument Corp. Scientific Glass Apparatus Company , Inc . Sherwood Medical Industries, Inc . Shimadzu Seisakusho, Ltd. Techne Incorporated Technical Operations, Inc. Testing Machine, Inc. Texas Instruments, Inc. Industrial Products Div. Thermometer Corporation of America Arthur H. Thomas Company The Torsion Balance Company Henry Troemner, Inc. Cahn Division Ventron Instruments Corp, Voland Corporation West-Glass Corporation Manufactures TECAM density gradient column . Manufactures precision pressure equipment which may be used as part of a system to measure volume of an unknown . TECAM density gradient column for measuring density of small solid samples with precision approaching + 0.0002 g/ml. Manufactures model S-100 balance specifically for specific gravity determination . Manufactures Cahn density system which measures density of 1.5 mg sample to accuracy of six decimal places . 89 APPENDIX C DERIVATION OF AN EQUATION RELATING SPECIFIC GRAVITY, BULK WET DENSITY, AND WATER CONTENT Water content is defined as the weight of water in a sample divided by the weight of solids in the sample. W WC = ^ (1) s In that the weight of a material is equal to the volume of the material times its density, equation (1) becomes: VxD s s If the numerator and denominator of (2) are divided by the density of water at 4 C, equation (2) becomes D V x — w D, WC = f- (3) V x-^ s D, 4 D /D, is the specific gravity of water and can be assumed equal to one for this derivation. D /D. is the specific gravity of solids. Equation (3) then becomes s s Bulk wet density is defined as the weight of a wet sample divided by its volume : W BWD = ^ . (5) 90 Ignoring the dissolved salts, the total weight of water is the weight of solids plus the weight of water, and the total volume is the volume of solids plus the volume of water. Equation (5) becomes: W + W «r,~ W S ... BWD = ^— pp . (6) w s Again using the definition that weight equals volume times density, assuming the specific gravity of water is one, and dividing the numerator and denominator of (6) by the density of distilled water at 4 C, equation (6) becomes: V + V x G w s s BWD V + V (7) w s \ The density of distilled water at 4 C is one gram per cubic centimeter, and equation (7) is simplified to: V + V x G BWD - "v ;y S (8) w s Dividing the numerator and denominator of equation (8) by V results in : V 1 + Gs x ^ BWD = — £ (9) w Equation (4) may be directly substituted into equation (9) to obtain: 1 + wc BWD ~ (10) w 91 Equation (4) may be rearranged in the form: V V WC x G w s (11) and equation (11) may be substituted into equation (10) to form: 1+^ BWD = ^ (12) 1 + WC x G s Equation (12) may be solved for G to obtain: G = BWD s 1 + WC - (BWD x WC) ' v ' Symbols used in this derivation are: WC = water content (expressed as a percentage) W = weight of water (grams) w W = weight of solids (grams) D = density of water (grams per cubic centimeter) w D = density of solids (grams per cubic centimeter) D, = density of distilled water at 4 C (grams per cubic centimeter) G = specific gravity of solids V = volume of water (cubic centimeters) w ' V = volume of solids (cubic centimeters) BWD = bulk wet density (grams per cubic centimeter) W = total weight of solids and water (grams) V = total volume of solids and water (grams). APPENDIX D COMPUTER PROGRAM This appendix contains a computer program for the calculation of specific gravity using bulk wet density and water content. The pro- gram also compares the computed value with the specific gravity by actual determination. 93 o < z 2: or. c c z 3: a; O LLI > < o or LU K LU o z o > a z o CO — Z arc 2 >3" O ~> 2" »-•-.-. ZOO or>z>xz _j2i-><<>— LU u_ u- uj o o oj t— or qtol 3"H Z OOOOO XLU U-U )*-Z n II ii — i-OU-O (-MOvTvLLLL \— — t z •— a a. ex *: or Ocjcjuolo<_jlu o cco ii ii c0< Z^Z I < < II .-< — * •— I- OCJOOCOO. 33 IT 00 < Q a a o < oo r »■ » * IS • ceo tMLL •> • hC ►— OU- ^ro cc » rvi • •~o O— I ► LL t-l •■ wfl O e •O C\J,-« ZIL Of\j z< CJfNJQ. * -O c\jr\j-j:_j_i + J"00 ► **"» «— i f\l ^h OO _J - oroiiOZ OtU. COOiU."—OLU 94 APPENDIX E COMPUTER OUTPUT FOR NCEL DATA The computer output for the Naval Civil Engineering Laboratory data is contained in this appendix. Specific gravity values were determined by the computer program in Appendix D and the air comparison pyenometer. Median diameters are in millimeters. A zero reading in the median diameter column indicates that no grain size analysis data was available for that interval. 95 u. >to era? 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IT. »c sO i^ o >o C\j <\J J >} CTf<~>CC IT ^rf>Oh • • * • c f\j ro r\i rvj f\j cc ZlL CJ u <: O coc oco cr J vfr • ••••• ococoo ITMf > »o *- ' cr • • • • • JZ cr o >*■ IT' LfMTv »-h (*"> r- -c r>- f- r- cc • * • e • • f >j-fvi • • • • • a cr C'uj L. h- Z I I I I I I o»o1 at ar r c z- cu c I c cr o i c u < a u C Or O*" I c I a z- 108 APPENDIX F COMPUTER OUTPUT FOR HYDROGRAPHIC OFFICE DATA The computer output for the U. S. Hydrographic Office data is con- tained in this appendix. Specific gravity values were determined by the computer program in Appendix D and the bottle pycnometer method. Median diameters are in microns. A zero reading in the median dia- meter column indicates that no grain size analysis data was available for that interval. 109 f-r ^^o — I e « * C <_OCO 0(\ «o«tfvo^'f ccr->t»of^fN! ir>0'>t<^>0fr,ocvcr«coc^iu,icr Nh(^hChhOOOOOCC c ococcccocococ O >0 CT OCOOOCL«— "»f»-lO",-l(\J 00 r-* o a «-i f- C-. 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X <3 u K - • r t- — - r- \y 5" LT a: < vO ro 3 »-( o a rj o u\ i/> o o o » " 2 7 c o u. c to u. fvj r*> a »— « c> (Nl C\J > _J t 3 ^4' o iri a c. o o oo O o o~ a 6 or L. a t~ Ui rr c a C Dr o 120 »~ o < a <\i fM »-» CC >0 IT »o o C t- iXIQC Ct'-' .JUJU DC QO CC < rJSh ry :roo Li r\j <\» f\l a «• r- m © «o o p» » rv o 0C' f* o o LTi o vfi o ^ o 2" a a K z> < c M a. > P U.J UJ KJ c t- M z uo Q UJ a £ u. < *- _J a «r 0 2- 2 '..U S < <■ a < U. t- h- i/-, > C) UJ Of < r-t CT* r> r— 1 o o c o UJ i/" C' O O . z Z c a < < *- IX Of T < > a. o (/> u_ r^ >- (•1 c IA 3 CL c "" > Of 6 o (X O 2 Uj 2 U-i •— i ■2 r h- k UJ *~ cp 3: l/l U' or m o m * a o o O i^ . o c c a c y H2 l/> 121 BIBLIOGRAPHY Beckman Instruments Application Data Sheet P-8071, Two Techniques for Determining Densities of Barite Ores, Beckman Instruments, Inc., 1960. Beckman Instruments, Inc., Beckman Instructions - Model 930 Air Com- parison Pycnometer, p. 1-12, 1965. Berman, H., "A Torsion Microbalance for the Determination of Specific Gravities of Minerals", The American Mineralogist, v. 24, p. 434-440, 1939. Canada, D. C. and Laing, W. R., "Use of a Density Gradient Column to Measure the Density of Microspheres", Analytical Chemistry, v. 39, May 1967. Dixon, W. J., Biomedical Computer Programs, University of California Publication in Automatic Computations No. 2, University of California Press, 1968. Frondel, C, The System of Minerology, 7th ed . , v. 3, Wiley, 1962. Gregg, S. J., The Surface Chemistry of Solids, 2nd ed . , p. 269, Reinhold Publishing Corporation, 1961. Grim, R. E., Clay Minerology, p. 313-314, McGraw-Hill, 1963. Gruner, J. W. , "Densities and Structural Relationships of Kaolinites and Anauxites", American Minerologist , v. 22, p. 855-860, 1937. Joyce, R. J., "Purgable Air Comparison Pycnometer", The Analyzer, v. 2, p. 11-12, October 1961. Kerr, P. F., et al., Preliminary Reports, Reference Clay Minerals Research Project 49, American Petroleum Institute, 1951. Kraus , E. H., Hunt, W. F., and Ramsdell, L. S., Mineralogy , 4th ed . , p. 107-108, McGraw-Hill, 1951. Lib oratory Soils Testing, EM 1110-2-1906, Headquarters, Department of the Army, Office of Chief of Engineers, p. IV- 1 , 10 May 1965. , T. W. , Soil Testing of Engineers, p. 15-19, Wiley, 1951. Lambe, I. W . , "How Dry is a Dry Soil?", Proceedings of the Highway Research Board, v. 29, p. 495, 1949. 22 Landy , R. A., and McGahan, J. F., "The Purgable Air Comparison Pycno- meter: Evaluation and Application", The Analyzer, v. 4, p. 9-10, 1963. Mclntyre, D. B., Welday, E. E., and Baird, A. K. , "Geologic Application of the Air Pycnometer: A Study of the Precision of Measurement", Geological Society of America Bulletin, v. 76, p. 1055-1060, September 1965. Meinhold, T. F. and Buckingham, R. G., "Resin-Density Analysis Time Trimmed 75%, Chemical Processing, v. 25, p. 152-154, January- June 1962. Ostle, B., Statistics in Research, 2nd ed . , The Iowa State University Press, 1963. Price, E., "Rapid Determination of Percent Reduction of Iron Ore", Engineering and Mining Journal, v. 165, p. 118-120, 1964. Procedures for Testing Soils, 4th ed . , p. 92-94, American Society for Testing and Materials, 1964. Shapiro, L. , "Rapid Determination of Powder Density of Rocks by a Sink-Float Technique", U. S. Geological Survey Professional Paper 650-B, p. B140-142, 1969. Tuul, J. and DeBaun, R. M., "Measurement of Skeletal Densities of High Surface Area Inorganic Oxides with a Gas Pycnometer", Analytical Chemistry, v. 34, May-August 1962. Twenhofel, W. H. and Tyler, S. A., Methods of Study of Sediments, 1st ed., p. 89-92, McGraw-Hill, 1948. Thewlis, J., Encyclopaedic Dictionary of Physics, v. 6, p. 618, Permagon Press, 1962. U. S. Naval Hydrographic Office Technical Report 106, Investigation of Deep-Sea Sediment Cores, Part II. Mass Physical Properties, by A. F. Richards, October 1962. Waterman, H. I. and Wolfs, P. M. J., "Accurate Measuring of the Density of Solids, Using Helium as a Gaseous Medium", Applied Scientific Research, v. 6, p. 372, 1957. Waterways Experiment Station Miscellaneous Paper Number 3-478, Evaluation of the Beckman Model 930 Air Comparison Pycnometer, by J. E. Mitchell, May 1964. 123 INITIAL DISTRIBUTION LIST No. Copies 1. Defense Documentation Center 20 Cameron Station Alexandria, Virginia 22314 2. Library, Code 0212 2 Naval Postgraduate School Monterey, California 93940 3. Oceanographer of the Navy 1 The Madison Building 732 N. Washington Street Alexandria, Virginia 22314 4. Professor R. J. Smith 1 Department of Oceanography (Code 58) Naval Postgraduate School Monterey, California 93940 5. LCDR J. C. Henderson 2 USS ALBACORE (AGSS 569) Fleet Post Office New York, New York 09501 6. Department of Oceanography (Code 58) 3 Naval Postgraduate School Monterey, California 93940 124 Si'iurit\ C'ltiisifu'jtmn DOCUMENT CONTROL DATA -R&D H\ > las w/n atmn of title, hod\ , t ahstrm t and hu/cxhi^ annotation must be entered when the overall report i s classified) NA* No *CTlVlTV(('iirpi>r«/rrtufAii)f) Naval Postgraduate School Monterey, California 93940 2a. REPORT SECURITY CLAtSIFIC : A T ION Unc lassif ied 2b. GROUP is i'oht r i t i f Specific Gravity Determination of Marine Sediments TSCRIPTIVE NOTES (Type ol report and. inc lus i ve da I en) Master's Thesis; April 1970 »u TmORiSi (First name, middle initial, last name) Joseph C. Henderson 6 REPORT CATE April 1970 Ba CONTRACT OR GRANT NO b PROJ f c t no DISTRIBUTION STATEMENT 7a. TOTAL NO. OF PAGES 125 7b. NO OF RE FS 28 9a. ORIGINATOR'S REPORT NUMBERIS) 96. OTHER REPORT NO(S) (Any other numbers that may be aasloned this report) This document has been approved for public release and sale its distribution is unlimited. II SUPPLEMENTARY NOTES 13 ABSTRACT 12 SPONSO RING Ml LI T AR Y ACTIVITY Naval Postgraduate School Monterey, California 93940 Accurate specific gravity measurements are required for the analysis of physical properties of marine sediments. Application of the bottle pyenometer technique, the standard determination method, is time-consuming, tedious, and perhaps subject to inaccuracies in the case of fine particulate matter. A review of methods currently in use was conducted to ascertain the present state of the art and reveal any new developments in this field. Specific gravity values for three operating modes of the air comparison pyenometer, two of which use helium, were compared with bottle pyenometer values for four test materials. The air comparison pyenometer determinations, regardless of operating mode, resulted in higher specific gravities than their counterpart i.ittle pyenometer values for kaolinite, montmori 1 lonite , and marine sediment samples. The use of helium as the comparison medium in the air comparison pyenometer appears to reduce the surface active characteristics of the colloidal material. Specific gravity determinations by all four test methods agreed very well for powdered quartz samples with a known specific gravity. DD FORM t NO V «s S/N 01 01 -807-681 1 1473 (PAGE 1) 125 Security Classification A-31408 Security Classification key wo R OS Specific gravity determination Marine sediments Air comparison pycnometer Bottle pycnometer technique DD ,F.r..1473 26 Security Classification J ONOn? S 1 0 7 1 2 117849 Thesis H4393 Henderson c-l Specific gravity determination of marine sediments. I a N 0 V 7 ? S 1 0 7 l 2 19 ine 117S49 Thesis H4393 Henderson c.l Specific gravity determination of marine sediments. thesH4393 Specific gravity determination o man liii'iiiiiiiiillllllllllllllH""" illlllllllllllllilliillllllllHIl™ 3 2768 001 91835 2 DUDLEY KNOX LIBRARY