API RECOMMENDED PRACTICE For TESTING OIL-WELL CEMENTS

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( f *«iiit iiitiiii«ti»i itti»ttiniiiif iti iii iaiiiiiiiBiiiitiiiiiEiiiBii**i»i iatiiiiitiiii*iaitiiaaiaiiiciiii«API RP 10BSeventh EditionJanuary 1958 "APIRECOMMENDED PRACTICEforTESTING OIL-WELL CEMENTSoAMERICAN PETROLEUM INSTITUTENew York, N . Y .Issued byAPI DIVISION OF PRODUCTION300 Corrigan Tower Bldg.Dallas 1, TexasPrice: 75 iMiiiiiiiim Copyright 1958 by American Petroleum Institute

2American Petroleum InstituteTABLE OF CONTENTSPage3ForewordSect.Sect.I : SamplingI I : Preparation of Slurry45Sect. I l l : Determination of Density of Slurry.6Sect.IV: Filter-Loss Test6Sect.V: Strength Tests8Sect.V I : Soundness and Fineness TestsSect. V I I : Thickening-Time TestsPressure Temperature Thickening-Time TestAtmospheric Pressure Thickening-Time Test—AAtmospheric Pressure Thickening-Time Test—B910101213NoteThis edition of RP 10B supersedes the 6th edition datedMay 1957. I t includes changes adopted at the June 1957meeting, which were reported in detail in Circ. PS 1109.This recommended practice was originally published inFebruary 1948, as Code 32, and reissued as the 2nd editionin June 1952. In June 1952, this code was transferred to thejurisdiction of the Committee on Standardization of OilWeil Cements, and redesignated RP 10B. The 3rd editionwas issued in May 1954, and the 4th edition in May 1955.I t was advanced to "standard" in June 1955. Further revised editions were issued in 1956 and May 1957.This publicationmay be reproduced in whole or inpart, except that the "OfficialPublication"monogram appearingon the outside may not be reproduced. All reproductionsshall carry thestatement,"Reproducedby permissionfrom API RP10B:RecommendedPracticefor TestingOil-WellCements." This permissiondoes not include the right toreproducethis recommendedpractice as aseparatepublicationfor resale or as a translation.Suchrightis granted only on specialauthorization.

RP 10B: Testing Oil-Well Cements3API RECOMMENDED PRACTICE FOR TESTING OIL-WELL CEMENTSForeworda. This recommended practice is under the jurisdiction of the A P I Committee on Standardization ofOil-Well Cements.Class C: Intended for use from surface to 6,000-ftdepth,* for conditions requiring highearly strength. Available in the regulartype (similar to ASTM C 150, type I I I )and in the high sulfate-resistant type.b. This recommended practice describes test procedures for the evaluation and definition of thosephysical properties of cements of special importanceto the oil and gas industry. Certain of these procedures are required methods of test under A P IStd 10A: Specification for Oil-Well Cements.Class N : Intended for use from 6,000 to 9,000-ftdepth,* for conditions of moderate temperature and pressure. Available in theregular type (having moderate sulfate resistance) and in the high sulfate-resistanttype.c. These procedures are applicable to the following classes and types of oil-well cement (see A P IStd 10A for specification requirements).Class D: Intended for use from 6,000 to 12,000-ftdepth,* for conditions of moderately hightemperature and moderately high pressure. Available in the regular type (having moderate sulfate resistance) and inthe high sulfate-resistant type.Class E: Intended for use from 6,000 to 14,000-ftdepth,* for conditions of high temperatureand high pressure. Available in the regular type (having moderate sulfate resistance) and in the high sulfate-resistanttype.Class A : Intended for use from surface to 6,000-ftdepth,* when special properties are notrequired. Available in regular type only(similar to ASTM C 150, type I ) .Class B: Intended for use from surface to 6,000-ftdepth.* Available in the regular type(similar to ASTM C 150, type I I ) forconditions requiring moderate sulfate resistance, and in the high sulfate-resistanttype.*These depth limits are based on the conditions imposedby the casing cementing: well-simulation tests (Schedules1-9, incl.), and should be considered as approximate valueB.Class F: Intended for use from 10,000 to 16,000-ftdepth,* for conditions of extremely hightemperature and extremely high pressure.Available in the regular type (havingmoderate sulfate resistance) and in thehigh sulfate-resistant type.

4American .Petroleum instituteSECTION ISAMPLING1. In order to secure a sample of cement which istruly representative of the lot in question, it isrecommended that the following cement-samplingequipment and methods be employed whenever possible.2. Apparatus. The following apparatus for sampling cement should be used:a. Sacked Cement. A tube sampler, as shown inFig. 1, should be used, i f possible, for samplingsacked cement.b. Bulk Cement. For sampling bulk cement, eitherof the following samplers should be used:I . A tube sampler similar to that shown inFig. 2 consisting of two polished brass telescopic tubes with registering slots whichare opened or closed by rotation of theinner tube, the outer tube being providedwith a sharp point to facilitate penetration.The length should be appropriate to thevessel from which the sample is beingcollected.TABLE 1WEIGHT OF TEST SAMPLESQuantity forSingle Test,Method of Testmin., lb.Quantity forCompleteTests, min., lb.Soundness1Fineness1Thickening TimeAtmospheric PressureTest A3Atmospheric PressureTest B6Pressure Temperature.2Tensile strength2 (per gang mold)Compressive strength3 (per gang mold)111224123248I I . A small grocers scoop, for sampling duringloading or unloading operations.3. Procedure. The following procedure for sampling cement should be used:a. Sacked Cement. When using the sampler shownin Fig. 1, the Bates valve in the upper righthand corner of the sack should be opened, thesampler inserted diagonally, and the thumbplaced over the air hole. The sampler shouldthen be carefully withdrawn. When i t is impossible or not feasible to sample cement with thetube sampler, every effort should be made tosecure a representative sample from the lot ofcement in question, be i t large or small. Aminimum of one sample from each 50 sacks(or less) is desirable. The sample should thenbe placed in an air-tight container, preferablymetal, and kept there until immediately beforetesting is started.b. Bulk Cement. The various procedures given i nthe latest edition of ASTM C 183*: Method ofTesting Hydraulic Cement, should be used forthe sampling of bulk cement.4. Size of Sample. The minimum weights of cement required for test purposes are given in Table 1.The total weight of sample collected should not beless than 25 per cent i n excess of the amount required for the tests to be conducted.*ASTM standards referred to herein are available fromAmerican Society for Testing Materials, 1916 Race St.,Philadelphia, Pa.H8-A-I IAPPROX. VOL.* 19.6 CU.IM.FIG. 1TUBE SAMPLER FOR SACKED CEMENTGOZDFIG. 2TUBE SAMPLER FOR BULK CEMENT

RP 10B: Testing Oil-Well Cements5SECTION IIPREPARATION OF SLURRYterials. The materials retained on the screen should beweighed, the weight recorded as a per cent of the totalcement sieved, and a notation made as to its characteristics, after which i t should be discarded.Apparatus5. Scales, The indicated load on scales should beaccurate within a tolerance of 2 g for loads of2000 g or more, and within 0.1 per cent of the indicated load for loads smaller than 2000 g, exceptthat for new scales the tolerances on accuracy shouldbe one-half of these values. The sensibility reciprocalshould not be greater than twice the permissibletolerance on scale accuracy.10. Mixing Water. For reference tests, freshlydistilled water or distilled water essentially free ofCO2 should be used. For routine tests, any normalpotable water may be employed. The mixing watershould be measured in a graduated glass cylinder(see Par. 7) or weighed by means of scales andweights (see Par. 5 and 6).6. Weights. Weights should be accurate within thetolerances shown in Table 2, except that new weightsshould be accurate within one-half of such tolerances. On beam-type scales where the weights areon the beam, the indicated weights should conformto the requirements given in Par. 511. Temperature of Water and Cement. The temperature of the water prior to mixing should be80 5 F and that of the cement should be 80 10 F.12. Water Percentage. The water percentage byweight to be added for each class of cement shouldconform to the values given in Table 3. No watershall be added to compensate for evaporation, wetting,etc.TABLE 2PERMISSIBLE VARIATION IN WEIGHTSe-Variation,Plus or Weight,TABLE 3CEMENT SLURRY COMPOSITION12345WaterAr Required QuantityPercentto Yield 750 mlage byGal.of Slurry1*VAPI ClassWt. ofperof CementCementSackg. water g. cementA and B465.19444965C566.32479855N, D, E, and F404.5142010507. Graduated Glass Cylinders. Graduated glasscylinders should be large enough to measure anddeliver, in a single operation, the required volume ofmixing water, at 20 C (68 F ) . The variation in volumeshould not exceed 0.2 per cent. The graduationsshould be subdivided to at least 5 ml. The main graduation lines should be complete circles, and should benumbered. The intermediate graduations should extend around a minimum of one-fifth of the circumference, and the smallest graduations should extendaround a minimum of one-seventh of the circumference of the cylinder.NOTE: The addition of bentonite to cementrequires that the amount of water be increased.It is recommended, for testing purposes, that4.5 per cent water be added for each 1 per centbentonite in classes A, and B, and C, and S.8 percent water for each per cent bentonite in classesN, D, E, and F cement. For example, a class Acement slurry having a normalwater-cementratio of 46 per cent, to which is added 8 per centbentonite, will require an increase in watercement ratio to 59.5 per cent.8. Mixing Device. The mixing device for preparation of cement slurries shall be a 1-qt size, two-speedWaring Blendor. This is a propeller-type high-speedmixer capable of rotating at 4,000 rpm or greater atno load on "slow" speed, and 10,000 rpm or greaterat no load on "high" speed. The propeller blade andmixing container (1-qt) shall be constructed of corrosion resistant metal.13. Mixing of Cement and Water. Mixing of thecement and the requisite percentage of water at thegiven temperature shall conform to the followingmixing procedure:The required quantity of water shall be placed inthe mixing container, the mixer turned on "slow"speed, and the cement sample added in not morethan 5 sec. After all of the cement has beenadded to the water, the cover shall be placed onthe mixing container and stirring shall be continued at "high" speed for 35 sec.Procedure9. Screening. The sample of cement to be testedshould be passed through an 840 micron (No. 20)sieve meeting the requirements given in the latestedition of ASTM E 11: Sieves for Testing Purposes,in order to break up lumps and remove foreign ma-I14. Volume of Slurry. The volume of slurry in themixing container shall be 750 ml.

6American Petroleum InstituteSECTION IIIDETERMINATION OF DENSITY OF SLURRY15. Apparatus and Calibration. Cement slurrydensity should be determined by the use of any accurate instrument, such as a hydrometer or mud balance as described in A P I RP 29: Recommended Practice for Standard Field Procedure for Testing Drilling Fluids.16. Procedure. The procedure for using a hydrometer or mud balance should be as recommended inthe latest edition of A P I RP 29 except that theslurry, after being poured into the hydrometer ormud-balance cup, should be puddled 25 times toeliminate any air that may be entranced in theslurry.SECTION IVFILTER-LOSS TEST(Tentative)17. Apparatus. The following apparatus should beused.a. Filter Press. The filter press should consist of aframe and cylinder assembly similar to thatshown in Fig. 3. The cylinder should have aninternal diameter of 3 .07 in. and a height ofat least 2% in. The cylinder assembly should beconstructed of materials not affected by alkalinesolutions and so fitted that a pressure mediumcan be conveniently admitted into and bled fromthe top. The bottom of the cell should be closedby a bottom cap with a drain tube and necessarygaskets to provide an effective seal. The filtration area should be 7.1 sq in. The entire assembly should be supported in a convenient stand.b. Pressure Medium. Pressure should be suppliedby compressed air, nitrogen, or any other safeand adequate means of maintaining constant gaspressure.c Filter Medium. The filter medium should be28 x 500 Dutch Twill Weave stainless steelmetallic filter cloth with a stainless steel binderor a 325-mesh U S Standard Sieve Series screen! (ASTM E 11-39) supported by a 14-mesh SieveSeries screen, both fabricated from stainlesssteel into an integral unit.d. Graduated Glass Cylinders. The graduated glasscylinders should be large enough to contain andmeasure the expected volume of filtrate.18. Preparation of Filter Press and Slurry. Priorto placing the slurry in the press the filter press andcement slurry should be prepared as follows:a. Filter Press. The cell of the filter press shouldbe assembled dry.b. Slurry. When the cement slurry is prepared inaccordance with Sect. I I , i t is placed in the pressas quickly as convenient handling will allow. Thetime between cessation of stirring and application of pressure shall not exceed 2 min. Thetemperature of slurry should be determined indegrees Fahrenheit.c. Special Slurry. When the test is used on fieldprepared slurries or on pressure and/or temperature treated slurries, the method of preparation and handling shall be stated.

RP 10B: Testing Oil-Well CementsProcedure19. Placing of Slurry in Press and Commencing ofTest. The cell should be filled with at least 2 in. ofcement slurry, capped, and secured in the frame. A drygraduated cylinder should be placed under the draintube to receive the filtrate, the relief valve closed, anda gas pressure of 100 5 psi applied within 5 secafter the relief valve is closed.20. Test Period. The test period should be timedfrom the instant of initial pressure application. Filtrate readings should be taken at Vi, %, 1, 2, and 5min, and thereafter at 5-min intervals, until 30 minhave elapsed. I f dehydration occurs before the end ofthe 30-min test period, the elapsed time required todehydrate the sample should be observed. A t thecompletion of the test, the gas pressure should beshut off and the relief valve opened.21. Recording of Results. Record the initial temperature of the slurry in degrees Fahrenheit. Thevolume of the filtrate should be recorded as follows:7a. For 30-Min Test Period. Report the volume offiltrate as the fluid loss at 100 psi.b. For Short Test Periods. For slurries which dehydrate in less than 30 min, and tests of shorterduration than 30 min, a hypothetical 30-minfluid-loss value may be obtained for comparativepurposes by multiplying the quantity of filtrateat that time by 5.477 divided by the square rootof that time in minutes. This relationship isshown by the following equation:Q30 Qt x-v tWherein:Q30 the quantity of filtrate in 30 min.Qt the quantity of filtrate at time t.All computed 30-min fluid-loss values should beso noted and should not be construed as truefluid-loss values., PRESSUREINLETCYLINDERI GASKET FILTERMEDIUM GASKET[BOTTOMCAPIN5.477,TUBEFIG. 3TYPICAL FILTRATION T E S T E R

8American Petroleum InstituteSECTION VSTRENGTH TESTSNOTE: Procedures are given for both compressive- and tensile-strength testing. However,comparative tests indicate that the results oftensile-strength tests do not reflect the effect ofvariation in age of specimens and in temperatureof curing as well as do the results of compressive-strength tests.22. Apparatus. The following apparatus shall beused:a. Sieve: 840 micron (No. 20) woven-wire clothsieve, meeting requirements given in the latestedition of ASTM E 11: Specification for Sievesfor Testing Purposes.b. Specimen Molds and Strength-Testing Machine: Molds and testing machine for the tensile-strength test conforming to requirementsin the latest edition of ASTM C 190: Method ofTest for Tensile Strength of Hydraulic-CementMortars. Molds and testing machine for the compressive-strength test conforming to the requirements in the latest edition of ASTM C 109:Method of Test for Compressive Strength ofHydraulic-Cement Mortars.c. Base and Cover Plates: Plate glass or non-corroding metal plates Yi-ia. thick, approximately4 in. wide, and 12 in. long.d. Water Curing Bath: A curing bath or tankhaving dimensions suitable for the completeimmersion in water of ASTM tensile or compressive molds and operable within 3 F of theprescribed test temperatures. The bath shallhave a suitable agitator or circulating system toinsure a uniform bath temperature. The twotypes of water curing bath are as follows:I . A non-pressure vessel suitable for curingspecimens at temperatures of 180 F or less.I I . A pressure vessel suitable for curing specimens at temperatures up to and including350 F, and at pressures that can be controlledbetween 0 and 3,000 psi. The vessel shallhave sufficient heating capacity to raise thetemperature uniformly from 80 to 300 F in100 min.e. Cooling Bath: A bath in which the specimen tobe cooled from the curing temperature, can becompletely submerged in water maintained at80 F, 5 F.f. Thermometers:I . Thermometer, range 0-220 F, with minimumscale divisions not exceeding 2 F, for use innon-pressure type vessels.I I . Pyrometer or thermometer, range 0-400F, with minimum scale divisions not exceeding 5 F, for use in pressure type vessels.g. Puddling Rod: A glass puddling rod approximately 8 in. in length and U, in. in diameter.h. Cup Grease: Cup grease, grade No. 2.i . Asphalt: Asphalt f o r use in sealing specimenmolds, having a softening point above 180 F.Procedure23. Preparation of Slurry and Molds. The cementslurry and molds used for strength-test specimensshall be prepared prior to placing the slurry in themold as follows:a. Slurry. The cement slurry shall be prepared inaccordance with Sect. I I .b. Molds. The interior faces of the molds and thecontact surface of the plates shall be thinlycovered with cup grease. The contact surfacesof the halves of each mold shall also be coatedwith cup grease to make the joint water tightwhen assembled. Excess grease shall be removed from the interior faces of the assembledmolds, and the molds placed on a thinly greasedplate or sealed to the base plate with asphaltheated to a pouring consistency and applied tothe exterior contact lines of the molds and baseplates. In the event that cup grease is used, i tis necessarv that i t be applied to the exteriorcontact line of the mold and the base plate.24. Placing of Slurry in Molds. The slurry shallbe placed in the prepared molds in a layer equal toone half of the mold depth, and the layer puddled 25times per specimen with a puddling rod. The slurryshall be placed in all the specimen compartmentsbefore commencing the puddling operation. On completion of the puddling of the layer, the remaining slurry shall be stirred to eliminate segregation,after which the molds shall be filled to overflowingand puddled as f o r the first layer. After puddling, theexcess slurry shall be struck off even with the topof the mold, using a straightedge. Specimens in moldswhich show evidence of leaking shall be discarded.A greased cover plate shall be placed on top of themold.25. Curing Periods. The curing period is the elapsedtime from that of subjecting the specimen to temperature in the curing vessel to that of testing the specimen for strength.a. For specimens cured at atmospheric pressure,the curing period starts when specimens areinitially placed in the curing bath, immediatelyafter slurry has been placed in the molds. Thecuring period ends when specimens are testedfor strength.b. For spec

RP 10B: Testing Oil-Well Cements 3 API RECOMMENDED PRACTICE FOR TESTING OIL-WELL CEMENTS Foreword a. This recommended practice is under the juris diction of the API Committee on Standardization of Oil-Well Cements. b. This recommended practice describes test pro cedures for the evaluation and definition of those

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