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Analysis of' Mudcake Structures Formed Under Simulated Borehole Conditions Albert Hartmann, * SPE, Technical U. of Clausthal Mustafa Ozerler, * * Inst. of Petroleum Research Claus Marx, SPE, Technical U. of Clausthal Hans-Joachim Neumann, Inst. of Petroleum Research Summary. Tiny pieces of filter cake were shock-frozen and broken while immersed in coolant. The specimens were studied with scanning electron microscopy (SEM) in both freeze-dried and frozen-hydrated stages. These techniques were used to show that the original structure of the filter cake is preserved. The investigation covered filter cakes of four different drilling fluids with respect to fluid loss data and thermal and chemical degradation. Honeycomb structures of bentonite containing drilling fluids were also found in the resultant filter cakes. The investigation showed that gel strength of the drilling fluid exerts a considerable influence on dynamic filter-cake structures. Introduction Both borehole stability and formation damage are functions of the fIltration behavior of drilling fluids. The fIltration behavior depends upon, among other things, the structure of the filter cake. Param- eters affecting filter-cake structure are type and alteration of the drilling fluids and filtration conditions (static or dynamic). I To date, knowledge of fIlter-cake consistency has been based on theo- retical considerations and conclusions from fluid loss data. 2,3 A single-handed evaluation from these parameters can sometimes result in different interpretations. The use of SEM for the study of samples with a high water content, such as filter cakes, requires sophisti- cated and thoroughly proven preparation techniques. 4 The appli- cation of shock-freezing and freeze-drying, originally used in biology and medicine, allows the use of SEM in drilling fluid tech- nology.5,6 A combination of SEM study of filter-cake structures with the evaluation of experimentally determined fluid loss data leads to a better understanding of the basic principles of fIlter-cake buildup and formation damage. This paper gives an SEM-aided description of filter cakes of different drilling fluids with respect to fluid loss data as well as thermal and chemical degradation. Test Program The test program is illustrated in Fig. 1. Two freshwater- and two saltwater-based drilling fluids were subjected to chemical or thermal prestressing or both. Filter-cake buildup was then conducted stati- cally on filter paper, in accordance with API RP 13B, dynamically on Bentheim sandstone (porosity = 20 to 24 %; permeability = 1.5 to 2.5 ILm2 , average pore radius =' 15 ± 7 ILm). For the subsequent structural analyses with SEM, the filter cakes were treated with a special preparatory technique. The problem was to elucidate the relationships between filter-cake structure and the type of drilling fluid, the previous history of the drilling fluid, and the type of filtration. Drilling Fluids, Both the compositions of the drilling fluids used and the sequences of their preparation are shown in Table 1. The drilling fluids were mixed with paddle stirrers. A high-speed stirrer was used for the preparation of the saltwater drilling clay (SWDC) suspensions (preponderantly attapulgite). The clay and polymer components were prepared separately. After a hydration period of 24 hours, the clay suspension was added to the polymer solution. The drilling fluids were then subjected to chemical stress through the addition of CaCl2 ' 6H20, to thermal stress in the roller oven, or to both. After a final mixing time of 2 hours with 6OO-rev/min paddle stirrers, the rheological and fIltration parameters were deter- 'Now at Eurosond. "Now at Research Ins!. of King Fahd U. of Petroleum & Minerals. Copyright 1988 Society of Petroleum Engineers SPE Drilling Engineering, December 1988 mined with a Fann viscosimeter and an API filter press (Table 2). The corresponding parameters measured on the unstressed drilling fluids were used as reference values. A portion of each drilling fluid sample was deliberately allowed to deteriorate completely under intense stress. Circulation Test Facility, The investigation on dynamic filtration was conducted with a circulation test facility developed at the Inst. of Petroleum Engineering (see Fig. 2). According to the Hassler cell principle, a rectangular rock specimen (2) is mounted in a rubber sleeve (3) in an autoclave (1). The rubber sleeve is subjected to pressure by a hydraulic pump (4). The drilling fluid is drawn from the storage tank (5) with a reciprocating pump (6) and allowed to flow across the face of the rock specimen. The system pressure is imposed with a nitrogen-actuated pulsation attenuator (7). The resultant differential pressure provides the driving force for the dy- namic fIltration through the Bentheim sandstone saturated with 1.5 % KCI solution. The fIltrate volume is measured as a function of time with an electronic balance (8) and transmitted through a digital- analog converter (9) to a strip-chart recorder (10). The technical specifications on the facility and the experimental conditions are shown in Table 3. The advantages and disadvantages of this setup, as compared with those for conventional Hassler cells charged with cores, are (I) simu- lation of the borehole conditions by upward, tangential flushing of the rock specimen; (2) homogeneous filter-cake buildup over the entire rock surface; (3) no dissolution of nitrogen in the drilling fluid; (4) time-consuming and expensive preparation of the rock plates by precise, plane-parallel sawing; and (5) no information con- cerning the thickness of the filtration zone. SEM Preparation Technique Theoretical Basis, To study the structure of filter cakes with SEM, the samples, which contain more than 70% water, must be dried before examination. Although several methods can be used to dry samples with a high water content, 7 the experiments carried out in the framework of this research program have shown that a com- bination of shock-freezing and freeze-drying is suitable. 8 The filter cakes can also be observed on SEM without freeze-drying, as so- called frozen-hydrated specimens. This method requires some tech- nical preconditions, such as cold-stage sample transfer from the coating facility to the SEM equipped with a special cold-storage plant. 9 ,10 This technique allows direct viewing of frozen specimens. 7 In relation to this technique, freeze-drying is more conventional. Freeze-drying is the removal of water from frozen material. II The purpose of this procedure is the transition from the solid to the gaseous state by sublimation without passing through the liquid 395 Type of drilling fluid Prestressing of drilling fluid Build-up of filter cake Bentoni te - fresh water- r-Uns tressed Chemically stressed by the addition- ~tatically Chalk - fresh water- of 40 g CaCl,'6 H,O to 1000 g H,O (API-filter press) in the drilling fluid - - Attapulgite - salt water- -Thermally stressed by 16 hours'_ exposure to 1S0 ll e L-oynamically (Circulation device) Attapulgite-bentonite -_ I-Chemically and thermall salt water stressed Fig. 1-Test program. TABLE 1-COMPOSITIONS OF DRILLING FLUIDS Type of Drilling Fluid Composition Bentonite/freshwater 1,000 9 H2O+ 60 9 sodium bentonite 5 9 sodium carboxymethylcellulose Chalklfreshwater 1.000 9 H2O+ 15 9 sodium bentonite 27 9 sodium carboxymethylhydroxyethylcellulose 15 9 potassium chloride 150 9 chalk 10 g'defoamer Attapulgite/saltwater 1,000 9 H2 0+ 55 9 attapulgite 38 9 starch 360 9 sodium chloride Attapulgite/bentonite/saltwater 1.000 9 H20 + 45 9 attapulgite 15 9 sodium bentonite 10 9 vinylamide/Vinylsulfonic acid copolymer, ammonium salt 360 9 sodium chloride TABLE 2-COMPOSITIONS AND TYPES OF PREPARATION OF DRILLING FLUIDS· Type of Drilling Fluid Bentonite/ freshwater Chalkl freshwater Attapulgite/ saltwaterAttapulgite/ bentonite/ saltwater Water Na·Bent. Na·CMC CMHEC KCI Chalk SWDC VSNA ~ ~ ~ ~ Jm. ~ ~ ~ 9,000 600 1.000 50 9.600 9 sodium bentonite suspension and 1.050 9 Na·CMC solution 2.250 150 7,750 270 2,400 9 sodium bentonite suspension and 8,020 9 CMHEC solution 150 1,500 10,000 550 ~~ ~ 3.000 150 2.500 100 4,950 9 SWDC suspension and 3.150 9 sodium bentonite suspension, addition of 2,600 9 VSNA solution "Na·Benl. = sodium bentonite. Na'(;MC ~ sodium carboxymethylcellulose. CMHEC m carboxymethylhydroxyethylcellulose. SWDC = saltwater drilling clay (preponderantly attapulgite). VSNA = vinylsulfonatelvinylamide. Starch NaCI ~ ~ 380 3,600 3.600 Mixing Time (hrs) 2 2 2 2 2 2 1 2 0.5 2 1 0.5 2 2 1 1 1 Note: The mixing was done with a paddle stirrer at 600 revlmin (Exception: The attapulgite suspension was prepared by a Hamilton Beach high-speed stirrer with 16.000 rev/min). Period of Hydration (hrs) 24 24 24 24 24 24 396 SPE Drilling Engineering, December 1988 1, Autoclave 2, Rock sarrole J , Rubber s I feve " PlJT1l un I t 5, Drilling fluid tank with heating devi ce 6, Piston DlJI'I) 7 , Pulsation attenuator 8, ElectronIc balance 9, 0lgltal-anal09 converter 8 10 , Strip-chart recorder Fig. 2-Clrculatlon lost facility. TABLE 3-TECHNICAL SPECIFICATIONS OF THE CIRCULATION DEVICE AND TEST CONDITIONS Maximal Temperature, ac 120 Operating pressure, MPa 10 Closure pressure, MPa 15 Backpressure, MPa 10 Annular velocity, mls 00 During the Tests 20 0.7 2 o 0.6* Dimensions of the rock sample: 15)( 120x35 mm. Annular cross-sectional area: 15)( 10 mm.· 'getor. It>e txJildup oIlhe fi lt'" caka. state. Ice sublimation is a function of temperature and vacuum- the lower the temperature, the higher the vacuum required for the water to leave the sample. Freeze-drying is usually carried out at about 200 K [- 100"F] and at a pressure of 20 to 100 MPa [2900 to 14,500 psij .12 Lower temperatures diminish ice recrystallization but require much higher vacuum and/or longer drying times. The n«:cssary time for freeze-drying depends on the propenies of the samples-such as size, shape, the amounts of free and bound water, and the ratio of fresh to dry weight. l3 Allowing the specimen to reach ambient temperature gradually under vacuum before it is re- moved from the freeze-dryi ng device is imponant for the procedure. Several authors show that shrinkage does bke place during the freeze-drying process on medical and biological specimens. l . iO• t2 Therefore, filter cakes were investigated after freeze-drying and on frozen-hydrated specimens (Figs. 3 and 4). The characteristic honeycomb structures formed by the bentonite platelets 14. t~ are clearly evident. The results of both tests have shown that there are no significant differences in filter-c.ake structure. This can be at- tributed to the fonn sbbility of aqueous clay/polymer systems. For the structural analysis with the help of SEM , both techniques are suitable. Cooling the specimens as rapidly as possible is neccliS8ry to avoid ice-crystal-growth damage during tne shock-freezing process. The specimens should be cooled down to 133 K [ - 220"F] within a few millis«:onds to obtain ice crystals only in microcrystalline or in glassy fonn (vitrification) . For optimal shock-freezing, the specimens must be as small as possible. The thermal contact with the coolants has to be good and the temperature gradient high. SPE Drilling Engineering. December 1988 Fig. 3- Freeze-drled tIIter cake of unstressed bentonitefCMC drilling fluid. 397 ~se I ~ .. ~ , OW .... ~"hO< 00' . Fig. 5-Scl'lematlc presentation 01 rshock-lreezlng and freeze- drying technlquel. - 20 ~ > -~ § u ~n o Itr, .. <!)o;h • • . Hre .. I!Ither • . Itr ... 1 ,h •• . • no trIer •. ttre •• 5 10 IS Time t 20 25 30 In min Fig. 6-Stltlc IIItrlte volumes 01 bentonltelfreshWlter drill- Ing fluid VS. time with respect to prestressing. Fig. 7-Statlc filter cake of unstressed bentonite/freshwater drilling lIuld. Several coolants with low melting points-such as propane ( 133 K [ - 220°F I) . isopentane ( 11 3 K [-256°F]) . Freon 12 (123 K [ - 238°FJ). or 2' methyll)utane ( 11 3 K [ -256°F))--can he used for shock. rreezing.4 These coolants must be cooled with the help or liquid nitrogen. Liquid nitrogen is not suitable for direct plunging ortne specimens. With a liquid·nitrogen coolant bath. tne fonnation of an isolating gas mantle impairs the thennal contact around the specimen (Lcidenfrost"s phenomenon). Liquid nitrogen can be used liS coolant only if subcoolcd to 63 K [ ~346°F]. where solid nitrogen noats in liquid nitrogen. 398 Fig. 9-8tatlc IlIlar clke 01 unatressed chalk/freshwater drill- Ing fluid. ~ " ~c s trl •• C 'lim . ' tr ' lI ;; 160 I!Itl'ler," . t tt ... X en' .. . '~CI t~. r," . ~ 120 I trlsl -' ~ I~ ~ 80 ~ --- '0 --~ > --~ 5 10 IS 20 25 30 - i! Time t in !!li n u Fig. 10-Statlc filtrete volumes of chalkl1relhwater drilling lIuld VI. time with respect to prestressing. ApplK-lition of Method. Thc filter cakes were broken or cut inlo liny pieces and plunged into ~ubcooled liquid nit rogen or in 2- melhylbutane cooled by liquid nitrogen (Fig. 5). After shock- rreezing. the samples were broken inside the coolant bath again to have an undisturbed surface for the SEM study. In the next step, the specimens were transferred while still covered with liquid nitrogen or 2-mcthylbutane to the precooled cold stage of the freeze- drying device. Freeze-drying occurred in IWO phases: (I) ini tial drying phase with sublimation at the ~ urface at 200 K r - IOO"F] and (2) final drying phase at a temperaturc of about 253 K [- 4 °F1. SPE Drilling Engineering. December 1988 FIg. 11-Statlc tIIter cake 01 thermally streased chalk/fresh· water drillIng fluid . Freeze-drying time varied from a few hours to several days de· pending on the specimen size and watcr content. The freeze-dried filte r-cake specimens were finally COOted with an electrical con- ducting layer and suJ(!ied with SEM. R.sults .nd Discuaalon Static Filter Cakes or Prestressed Drilling Fluids. Befl- tQn jteIFresh""ater DriJling Flujd. The filtration volume is plotted as a function of time for bentonite/freshwater drilling fluid in Fig. 6. Because the protective colloid used. carboxymethylcellulose (CMC), is not stable toward divalent clItions. chemical stress that results from the addition of CaCl2 '6H 20 causes a substantial in- crease in the filtrate volume. This is reflected in the structural analyses perfonned on the filter cakes by SEM. In the unstressed case. the gel structures present in the drilling fluid are decisive for the texture (Fig. 7). The applied differential pressure of O. 7 MPa [101 .S psi] is not sufficient to disrupt the electrostatically mduced edge-to-face allachment between the bentonite platelets. The chemical prestressing of the drilling fluid resulted in complete dis- ruption of the characteristic honeycomb structure (Fig. 8). This process is associated with partial dehydration and coagulation of the bentonite particles (fact·to-face ~lIachment). 16 This resulted in enlargement of the effective-flow cross section within the filter cake SPE Drilling Engineering. December 1988 Fig. 13-Stallc IIIter cake 01 un.tressed attapulgltelsaltwatar drilling fluid (no saluratlon with NaCI). FIg. 14-Statlc filte r cake 01 unatreased al tapulgite/sallwater dril ling fluid . ~ e u c - 160 0 ~120 0 > ~ 80 • , - " -• > -• 5 § u 10 15 ~n lJ .tress <?cl'le •. stress [!Jtl'lerll. s tres s X c~ .... ~nd tl'ler •. ,tress 20 25 JO TIme t In min Fig. tS-Static IUlrale volumes 01 attapulglte/saltwater drill. Ing Iluid vs. t ime with respect to prestressing. 399 Fig. 17-Statlc !liter cake 01 unstressed attepulglte/bentonltel saltwater drilling fluid (no saturation with NaCI).and thus in an increase in filtrate volume. t7.18 A further deterio- ration of the filtralion p,r0perties is attributed to the conversion of Na-CMC to Ca-CMC. 9 The laner no longer exerts a sealing effect within the filter-eake struelure . Chalkl FreshwaJer Drilling fluid. The filter cake formed from chalk/freshwater drilling fluid presents an entirely different picture (Fig. 9). A characteristic feature is the presence of partially an- gular and partially rounded chalk particles of various siJ:cs, which cause a decrease in filtrate volume. in contrast to bentonite/fresh- water drilling fluid (compare Figs. IO and 6). Examination at high magnifications has indicated that the chalk particlcs are frequently coated with a polymer film, lose their sharp edges and fracture surfaces, and are progressively more strongly bonded together. The Structure-fonning bentonite platelets, whose honeycomb structures are in part still discernible, provide additional sealing. The chalk product used contains numerous skeletal remains of coccoliths, which lived in the sea as plankton. Thennal prestfCSsing of the drilling fluid does not seriously impair the rIlter--cake structure, as can be seen in Fig. I I; locaiiJ:ed honeycomb structures are still present even after subjection to thermal stress. This indicates the thermal stability of carboxymcthylhydroxyethylcellulose (CMHEC), the protcctive colloid used. A comparison of the filtration curves (Fig. 10) indicates only a slight increase in filtratc volume during thermal prestressing of the drilling fluid . AIWpulgite!Saltwalu Drifting Fluid. For the structural analysis of filter cake, it is often advisable first to visuaiiJ:e the individual Fig. 18-Statie fitter cake of unstressed attapulgitefbentonltei saltwater drilling fluid . Fig. 19-5talic filter cake 01 chemically and thermally stressed attapulgltelbentonlte/aaltweter drilling fluid. components. A 6% attapulgite/freshwater suspension is shown at high magnification in Fig. 12. The individual attapulgitc needles are clearly recognizable. A characteristic featu re is the pronounced matting of the needles to form bundles.2() The filter cake formed by the attapulgitelsaltwater drilling fluid beforc the addition of salt is illustrated in Fig. 13. Besides the attapulgite agglomeration, the structure of the filter cake is affected by the crosslinking action of thc starch used as a filtration control agent. The filter cake formed from the attapulgite/saltwater drilling fluid salted with NaCI all the way to saturation appears dense and compact (Fig. 14). The ab- sence of honeycomb structures is because of the weak tendency of the anapulgite needles to form gel SlfUctufCS.2l The salt crystals discernible at high magnification should be regarded as artifacts lhat arise upon recrystallization during freeze-drying. The lhermal degradation of starch causes an cxtremely high filtrate volume (Fig. 15) because the sealing action of the starch is then absent. t9 The filtcr cake is friable and highly permeable (Fig. 16). AttapufgilelBI!ntonitelSaftll'ater Drifting fluid. The lack of sufficent gel strength with the attapulgite/saltwater drilling fluid is because of a mixture of attapulgite and bentonitc in a ratio of 3: I . To ensure better thermal stability, a completely synthetic product was used as a protective colloid. The filter cake obtained from the unstressed at tapulgitefbentonite/saltwater drilling fluid before the addition of salt is depicted in Fig. 17. Despite the low bentonite content. the bentonite platelets affect the structure and constitute the macrostructure by edge-to-face attachment. The considerably SPE Drilling Engineering. December t988 -ro ~no 5 tr ••• <!>chell. stre" I!lthe ...... s tr ••• X ehe • . and tner •. stress 5 10 15 20 TIme t In min 25 30 Fig. 20-51811c filtrate volume. ol attapulglte/bentonlte/aalt- water drilling fluid VI. tlma with r.epecl to prestrening. Fig. 21-Oynamlc IIIter cake of chemically and thermally atrnsed anapulgltelbentonlteJultwlteT drilling fluid (no satu- ration with NaCI). smaller attapufgile needles form a microstructure al the walls of the honeycomb. Salting the drilling fluid with NeCl ali lhe way to saturation causes apparent th ickening of the honeycomb walls in the filler cake (Fig. 18), The cause of this behavior is the same as that described for the attapulgitefsaltwater drilling nuid . TIle com- bined prestressing causes disruption of the gel structures formed by the bentonite (Fig . 19) and thus a more pronounced increase in filtrate volume (Fig. 20). A possible explanation for pure pro- tective action by the thermally stable polymer is the low concen- tration in the initial drilling fluid . The polymer filament molecules become attached predominantly to the attapulgilc needles; conse- quent ly, the major pon ion of bentoni te remains unprotected during exposure to elevated temperature. The results are coagulation and dehydration of the bentonite and thus an increase in the effective- flow cross section. Dynamic Filter Cakes. Dynamic filter cakes from unst ressed drilling fluids of high gel strength containing bentonite do not ex- SPE Drilling Engineering. December 1988 Fig. 22-Dynamic filter cake 01 un,tre,sed attapulglte/salt· water drilling fluid . Fig. 23-Dynamlc !liter cake of bentonite suspension treat- ed with thinner. hibit appreciable structural differences in comparison with the cor- responding static filter cakes. A structural orientation. which might pos.~ibly be expected to occur in the direction of flow for the drilling fluid. depends on (I) shear stress in drilling fluid, (2) differential pressure gradient , (3) extent of hydration of bentonite panicles. and (4) intensity of gel structures in drilling fluid . During the investigation, the gel strength of the drilling fluids was impaired by chemical or tncrnlal prestressing or both. The filter cake fonned from 3ttapulgitelbcntonitelsal!water drilling fluid before salting with NaCI and after the combined prestressing is shown in Fig. 21. A structural orientation within the fillCrcake corn:sponding with the morphology of the rock surface is clearly evmnt. Also. for fil ter cakes of unstressed drilling fluids. an orientation of the solids in the drilling fluid can occur in the direction of flow if the drilling flu id exhibits a very low gelstrength---e.g., in the case of an attapulgi te/saltwater drilling fluid (Fig. 22). Borst and SheilS studied the effect of adding thinner to drilling fluids with SEM. For examining the e ffect of the gel strength on the filter-cake '01 TABLE 4-PROPERTIES OF 6%* BENTONITE SUSPENSION Plastic Bingham 10-Second Gel 10-Minute Gel API Fluid Viscosity Yield Point Strength Strength Loss (mPa·s) (dPa) Untreated 8 115 Treated with 5 g thinner per liter 14 14 of suspension • Mass content. structure during dynamic fIltration, a 6% bentonite suspension was deflocculated by conditioning with modified polyacrylate. The rheo- logical and fIltration parameters are given in Table 4. Examination of the SEM photographs yields the following results (Fig. 23). .1. Extremely thin filter cake. 2. Orientation of the solids in the drilling fluid in the direction of flow. 3. Fluidized structure in the proximity of the rock. 4. Good sealing action of the fIlter cake (compare fluid loss before and after the addition of the thinner in Table 4). The importance of the gel strength of the drilling fluid for the filter-cake structure has been confirmed by this experiment. Conclusions Based on the investigations conducted for visualizing and inter- preting filter-cake structures, the following conclusions have been reached. 1. Frozen-hydrating and shock-freezing with subsequent freeze- drying are processes well suited for preparing filter cake appropri- ately for SEM. 2. Using bentonite gives rise to a honeycomb structure within the filter cake.This is induced by the edge-to-face attachment of the bentonite platelets. 3. During cherr.ical and/or thermal overstressing of the drilling fluid, the bentonite platelets lose their structure-forming property through coagulation. 4. With the use of SWDC, the acicular clays form bundles within the filter cake. 5. A structural orientation in the direction of flow for the drilling fluid within the filter cake can be observed only if the gel strength has diminished within the drilling fluid. 6. The application of SEM in drilling fluid engineering does not replace but rather supplements fluid loss analyses. Acknowledgment The investigations have been performed within the framework of SFB 134 "Petroleum Technology-Petroleum Chemistry" at the Technical U. of Clausthal with funds provided by the German Re- search Assn. References 1. Peden, J.M., Arthur, K.G., and Avalos, M.: "The Analysis of Filtration Under Dynamic and Static Conditions," paper SPE 12503 presented at the 1984 SPE Formation Damage Control Symposium, Bakersfield, CA, Feb. 13-14. 2. Roloff, J: "Untersuchungen iiber die Filterkuchenstruktur bei der dy- namischen Filtration sowie iiber die Filterkuchenabtragung mit ober- fliichenaktiven und abrasiv wirkenden Waschfliissigkeiten," PhD dissertation, Inst. of Petroleum Engineering, Technical U. of Claus thai, Clausthal-Zellerfeld (1969). 3. von Engelhardt, W.: "Filterkuchenbildung und Wasserabgabe von Tief- bohrspiilungen," Erdal und Kohle (1953) 6, No.4, 191-95, 247-52. 4. Reimer, L. and Pfefferkorn, G.: Rasterelektronenmikroslwpie, Springer- Verlag, Berlin (1977) 250-52. 5. Borst. R.L. and Shell, F.Y.: "The Effect of Thinners on the Fabric of Clay Muds and Gels," JPT(Oct. 1971) 1193-1201. 402 (dPa) (dPa) (cm 3 ) pH Value 119 0 158 20 10.2 0 12 8.9 6. Porter, E.K.: "A Basic Scanning Electron Microscope Study of Drilling Fluids," paper SPE 8790 presented at the 1980 SPE Formation Damage Control Symposium, Bakersfield, CA, Jan. 28-29. 7. Beckett, A. and Porter, R.: "Scanning Electron Microscopy of Frozen- Hydrated Material," Protoplas1rUll11, Springer-Verlag, Berlin (1982) 28-37. 8. Hartmann, A. and Ozerler, M.: "Method for Investigating the Structure of Filter Cake from Drilling Fluids, ., Erdal-Erdgas-Zeitschrift (1985) 101, No.9, 283-86. 9. Schwartz, D.E.: "Scanning Electron Microscope-Cold Stage: Viewing Fluid Saturated Reservoir Rock," paper SPE 9248 presented at the 1980 SPE Annual Technical Conference and Exhibition, Dallas, Sept. 21-24. 10. Robards, A.W.: "Instrumentation for Low Temperature Biological Electron Microscopy," Laboratory Practice (1983) 3, 19-23. 11. Griesbeck, G.: "Gefriertrocknung in Labor und Produktion," Medizin- technik (1983) 103, No.6, 173-78. 12. Goldstein, J.I.: Scanning Electron Microscopy and X-Ray Microanalysis, Plenum Press, New York City (1981) 495-534. 13. Boyde, A. and Echlin, P.: "Freezing and Freeze-Drying Electron Microscopy," Proc., Annual Scanning Electron Microscopy, Chicago (1973) 759-66. 14. Wilson, M. and Pittmann, E.: "Authigenic Clays in Sandstones and Influence on Reservoir Properties and Paleonenvironmental Analysis, " J. Sed. Petrol. (1977) 47, No.3, 3-31. 15. Osipov, V.I. and Sokolov, V.N.: "A Study of the Strength and Defor- mation Properties of Clay Soils with the Help of Scanning Electron Microscopy," Bull., IntI. Assn. of Engineering Geology (1978) 17, 91-94. 16. van Olphen, H.: An Introduction to Clay Colloid Chemistry, John Wiley & Sons Inc., New York City (1966) 93-95. 17. Gray, G.R. and Darley, H.C.H.: Composition and Properties of Oil Well Drilling Fluids, fourth edition, Houston (1983) 293. 18. von Engelhardt, W. and Schindewolf, E.: "Zur Filtration von Ton- suspensionen," Kolloid-Zeitschrift, (1952) 127, No. 2/3, 150-64. 19. Thomas, D.C.: "Thermal Stability of Starch- and Carboxymethyl Cellulose-Based Polymers Used in Drilling Fluids," SPFJ (April 1982) 171-80. 20. Giiven, N., Leroy, L., and Lee, L.J.: "Reactions of Attapulgite and Sepiolite in High Temperature Drilling Fluids," Proc., Inti. Conference on Geothermal Drilling and Completion Technology, Albuquerque, NM (1981) 26/1-26/22. 21. Bulian, W. and Djahanschahi, H.: "Uber die Temperaturbestiindigkeit von salzgesiittigten Bohrspiilungen, " Erdal-Erdgas-Zeitschrift (1969) 85, 5, 168-89. 51 Metric Conversion Factors cp x 1.0* E+oo mPa's ft3/(min-ft) x 5.08* E-03 mls OF (OF-32)/1.8 °C OF (OF+459.67)/1.8 K in. x 2.54* E+Ol mm Ibf/loo ft2 x 4.788026 E-Ol Pa mL x 1.0* E+oo cm3 psi x 6.894757 E+oo kPa *Conversion factor is exact. SPEDE Original SPE manuscript received for review Oct. 5, 1986. Paper accepted for publication Nov. t 7, 1987. Revised manuscript received June 8, 1988. Paper (SPE t 5413) first presented althe t986 SPE Annual Technical Conference and Exhibition held in New Orleans. Oct. 5-8. SPE Drilling Engineering, December 1988