LABORATORY TESTING PROCEDURES MANUAL VOLUME III PORTLAND CEMENT Department of Public Works and Highways BUREAU OF RESEARCH AND STANDARDS February 1997TABLE OF CONTENTS Page FOREWORD VOLUME IIT ~ TESTING OF PORTLAND CEMENT 1, Determination of Density of Hydraulic Cement ------- 1 2. Determination of Fineness of Hydraulic Cement by the No. 200 (0.075-mm) Sieve = - = === - = - ~~ A 3. Determination of Fineness of Portland Cement by Air Permeability Apparatus =~ - --— = - ~~~ ~~ - 5 4, Determination of Normal Consistency of Hydraulic Cement =~ = Se ee a 5. Determination of Time of Setting of Hydraulic Cement by Gillmore Needle - - - -- ------ 15 6. Determination of Time setting of Hydraulic Cement by Vicat Needle ----------- - 7. Soundness Determination of Portland Cement by Autoclave Expansion ---- ~~ were eee an 8. Determination of Air content of Hydraulic Cement ---- 23 9. Determination of Compressive strength of Hydraulic Cement Mortars (Using 50 mm Cube specimens) - - 26 40. Determination of Loss on Ignition (#ydraulic Cement) ---- === ------ a a 11, Determination of Insoluble Residue (Hydraulic Cement) ~ =~ ---- ~~~ crescent on 12. Determination of sulfur Trioxide Content (iydraulic Cement) = = = eee eee Ea 13, Determination of Magnesium Oxide Content (Hydraulic Cement) = - =~ == = woe --- 8s 33DETERMINATION OF DENSITY HYDRAULIC CEMENT The value of specific gravity of cement is used in the design and control of concrete mixtures APPARATUS 1. Le Chatelier flak, Fig. 1 2. Kerosene free of water, or naphta, having a gravity not lighter than 62 API shall be used in the density determination. 3. Balance and weights PROCEDURES 2, Fil Le chatelier flask with kerosene, free of water, or naphta to a point on the stem between the zero and Inn mark. 2, Immerse the flask in a water bath of constant temperature, maintained at ambient temperature, for a sufficient time before making any reading, 3. Take initial reading. 4. Introduce into the flask the cement sample, at least 64 grams. 5. Remove air bubbles by gently rolling the flask with stopper and swirling occasionally. 6. immerse in water bath, then take final reading: CALCULATION: 1. ghe difference between the “first and the final reading Eepresents the volune of Liguid displaced by the mass of cenent sed in the test 2. Calculate the cement density, p, in g/en? as follows: ea ee 2 sneccicat ath Final reading - Initial reading NOTE 1 - The density in g/en? is numerically equal to specific gravityLE CHATELIER FLASK FOR DENSITY TEST figure 1eR RRRRERERERERERERRERR ERED DETERMINATION OF FINENESS OF HYDRAULIC CEMENT BY ‘THE NO. 200 (0.075-mm) STEVES APPARATUS 1 ‘PROCEDURE, Sieves, Standard No. 100 (150-um) or No. 200 (75-um) sieves conforming to the requirements of the AASHTO M 92, for Wire Cloth “Sieves for Testing Purposes. Wire cloth for standard sieves for cement shall be veven (not tyilled) from brass, bronze, or other suitable wire and mounted without distortion on a frame about 2 in. (50 nm) below the top of the frame. the Joint between the cloth and frane shall be smoothly filled with Solder to prevent lodging of the cement. The sieve frame shall be circular, @ in. (203 mm) in diameter and provided with a pan and cover. Balance ~ The analytical balance used in fineness determinations shall conform to the requirements of 4.1 of AASHTO T 105, for Chenical Analysis of Hydraulic Cement. Brush - A 1 or 1 1/2 in. (25 or 38-mm) brush with a 20 in. (250-mm) handle is a convenient size. Weights Place at least 50 grams cement sample on the clean, dry No. 0.075 mm sieve with the pan attached. Start sieving with » gentle wrist motion until most of the fine material has passed through the sieve and the residue appears fairly clean for a period of ¢ minutes Place the cover on the sieve and remove the pan. Then gently top the side of the sieve to dislodge dust adhering to the sieve. Brush also the underside of the sizve. Empty the pan and wipe it. Then replace the sieve on the pan, and Carefully venove the cover. Return any coarse: material that has been caught in the cover during the tapping to the sieve. Continue the sieving without the cover as described in procedure #2 for 5 or 10 min. depending on the condition of the cement. The gentle wrist motion involves no danger in spilling the Eesidue, which shall be kept well spread out on the sieve. Continuously rotate the sieve throughout the sieving. This open sieving may usually be continued safely for 9 min or more, but take care that it is not continued too long. Then replace the cover and clean, follcwing the same process as described in Procedure # 2. If the coment is in proper condition, there Should now be no appreciable dust renaining in the residue nor adhering to the sieve or panMake i-min tests as follows: Hold the sieve, with pan and cover attached, in one hand in a slightly inclined position and move it forward and backward in the plane of inclination; at the same time gentiy strike the side about 150 tines/nin against the palm of the other hand on the upstroke. Perform the sieving over a white paper. Return any material escaping from the sieve or pan and collecting on the paper to the sieve. After every 25 Strokes, turn the sieve about one-sixth of @ revolution, in the Same direction. Continue the sieving operation until not more than 0.05 g of the material passes through in 1 min. of continuous sieving. Then transfer the residue on the sieve to the balance pan, taking care to brush the sieve cloth thoroughly from both sides to ensure the removal of all the residue from the sieve. Then transfer the residue on the sieve to the balance pan. Brush the sieve cloth thoroughly from both sides to insure the Hemoval of all residue from the sieve SOMPUTATION : We, of residue (g) x 100 © Fineness = Ss We. of original sample (9)DETERMINATION OF FINENESS OF PORTLAND CEMENT ‘BY AIR PERMEABILITY APPARATUS STONIFICANCE : This method is intended for the determination of the fineness of Portland cement, in terms of the specific surface expressed an tater Surface area in square centineters per gram, oF square meters per kilogean APPARATUS 1. Blaine air permeability apparatus illustrated in Figure, 2, consisting essentially of the following parts? a) Permeability cet 2) Disk ©) Plunger. 4) Filter Paper £) Manometer 1iquie 9) Timer ‘CALIBRATION OF APPARATUS The calibration of the air permeability apparatus shall be made using the current lot of National Bureau of standards Standard Reference Materiey No. 114 and shali be at room temperature Determine the bulk volume of the compacted bed of powder by the mercury displacement meted as follows: a) Place two (2) filter paper diaks in the permeability cell, Pressing dovn the edges by a rod having a diameter saightly smaller than the cell until the disks are flat on the perforated metal disk, then fi11 the cell with mercury. >) Level the mercury with the top of the cell by slightly pressing a small glass plate against the mercury surface until the glace is flush to the surface of the mercury and rin of the cell. © Remove the mercury from the coli and weigh. @) Remove one (1) filter paper disk from the cell. using a trial quantity of 2.80 9 of cenent, compress the cenent in accordance with section (g) ‘Preparation of bed of cement with one Elites disk above and one below the sample. Into the unfilled space at the top of the cell, add mercury. Renove entrapped air and level off the top as before. Remove the mercury, then weigh Determine the bulk voiume occupied by the cement tothe formulael f) o where : Y= bulk volume of cement, cn? Ny = grams of mercury required te fill cell, no cement being in the cell ig = grams of mercury required to fill the portion of the cell not occupied by the prepared bed of cement in the cell b = Density of mercury at temperature of test, g/cm? (see table 2) Make two (2) trials, using separate compaction for each Neterminations and the average of the two values shall be used for subsequent calculations. the mass of the standard sample used for calibration shall be Tee aetuiced to produce a bed of cement having a porosity of 01500 + 0.005 and shall be calculated as follows: we pace where: a= grams of sample required p= density of test sample (for portland cement a value Of 3.15 Mg/n? or 3.15 g/cn® shall be used). v= bulk volume of bed of cement, cn? fe = desixed porosity of bed of cement (0.500 + 0.008) Prepare the bed of cen ¢ in accordat with the following 1. Seat the perforated disk on the edge in the permeability Gell, inscribed or marked face down. Place @ filter paper disk on the metal disk and press the tages down with a rod having a diameter slightly smaller fhan that of the cell. 3. Weigh to the nearest 0.001 g the quantity of cement Setgemined in accordance with section (£) and place in the cell 4. tap the side of the cell lightly to level the bed of cement 5) place a filter paper dick on top of the cement and ceeetess the cement with the plunger until the plunger Solar is in contact with the top of the cell. Slowly CCthareir the plunger a short distance and rotate about 90 Seg, Eepress and then slowly withdrav.i’ hy Perform the Permeability Test in accordance with the following 1) Attach the permeability cell to the manometer tube, making certain that an airtight connection 1s obtained and taking Gare not to disturb the prepared bed of cenent 2) Slowly evacuate the air in the one arm of the manoneter U- tube Until the liquid reaches the top mark, and then close the valve tightly: 3) Start the timer when the bottom of the minizcus of the manometer liquid reaches the second (next to the top) mark and stop when the bottom of the miniscus of liquid reaches Che third (net to the bottom), mark. Note the tine interval measured and record in’ seconds. Note the temperature of test and record in degree celsics 4) Th the callpeation of che instrument. Make at least three (3) trials on ‘a separately prepared beds of standard Sample. The calibration shall be made by the sane operator lho makes the fineness determination. ‘The cenent sample shall be at room temperature vhen tested. 2, The weight of sample shall be the sane as that used in the calibration test on standard sample. 3. Prepare the bed of cement in the same manner as that in section (3) 4. Perform the permeability test in the sama manner as that in section (h). CALCULATION Calculate the specific surface values in accordance with the following equations: 5st pos =specific surface of the test sanple, on’/g Specific surface of the standard sample used in calibration of the apparatus, cn?/g measured time interval, 5, of manometer drop for test sample (see Table 2) measured time interval, s, of manometer drop for standard sample used in calibration of apparatus (see Table 2) viscosity of air, poises, at the temperature of test of the test sample (see Table 1) viscosity ef air, poises, at the temperature of test of the standard sample used in calibration of the apparatus (see Table 2) cable 1 Density of Mercury, Viscosity of Aix in), and \/m at Given ‘romperature: Room Density of Viscosity of pare i ‘remper~ Mercury, air, a Va i avure, a dog ¢ i 16 13.56 0.0001788 0.01337 18 13155 00001798 0:01341, ; 20 1355 00001808 0101345, 22 13.54 o,o001823 0.01348 2 1354 ‘9.0004828 0.01352 i 26 13.53 0, 0001837 0.01355, i 28 13.53 0/on0i8e7 0101359 30 13.52 0,0001857 0.01363 32 13:52 0: 0001867 0,01366 ; 34 13/51 0001875 001370,TABLE 2 Time of Airflow T = time of airflow in seconds; \/T = the factor for use in the equations. ror Vor VWPor wo: For vr 26.10 26-4 5115 27 5:20 21-4 5.24 2 5.28 2e-% 5.34 29° 5139 16:38 29-4 5.43 Sd 7138 79-4 9.92 108 10139 188 12.57 208 14.42 30 5:48 55 7.42 80 8.94 309 10144 189 i2:61 209 14.46 30-4 5152 S$ar2 7.45 80-4 6.97 310 10:49 160 12/65 210 14049 315.57 $6 7.48 81 9.00 121 30.54 261 12.69 211 14.53 Bie 5.61 56% 7.52 G1-w 9103 112 10158 162 12-73 212 14.86 32 $.66 57 7:55 82 9:06 113 10/63 163 12-77 213 14.59 324 $.70 S74 7158 82-4 9108 11% 10169 164 12-81 214 isles 33° 5:74 58 7.62 83 9.11 115 10.72 168 12/85 213 Lele 33-4 5.79 S842 7.65 83-y 9.14 126 10.77 166 12.88 216 14.70 34 5.83 59 7168 84 917 127 0.82 67 12/82 217 14.95 34-4 5.87 59% 7.71 B44 9.19 118 10.86 168 12.96 218 Lace 35 5.92 60 7.75 85 9.22 119 10191 169 13:00 219 14.80 35-4 5.96 60-4 7.78 85-4 9.25 120 10:95 170 13-04 220 i489 36 6.00 61 7.81 86 9.27 121 11.00 171 19.08 222 14.90 3644 6.08 Gl 7:84 86-4 9.30 122 41105 172 13:1 224 14.97 37 | 6.08 62 7187 87 9.33 123 41.09 173 13.15 226 19.03 37-4 6.12 62% 7191 B74 91395 124 11/14 17d 13119 228 13.10 38 6.16 63° 7.94 88 9.38 125 11-18 175 13:23 230 18119 3-4 6.20 63-4 7.97 BB-4 9.41 126 11.22 176 13.27 232 15.23 33 6.24 64 | G100 89 | 9.43 127 41127 177 13:30 234 18.30 394 6.28 Git 0103 89-4 9.46 128 11131 178 13.34 236 13.36 40 6.32 65 8106 30 9.49 129 i136 179 13.38 238 13045 40-4 6.36 65-4 8.09 90-4 951 130 11.40 160 13.42 240 13043 42 640 66 6.12 91 9,54 331 11-45 161 13.45 242 15.56 4242 6.44 66% 6.15 91m 9:57 132 11149 182 13:49 244 18.62 42 6.48 67 8.19 92 9.89 133 11.53 183 13/83 246 islee 42-4 6.52 67-4 8.22 92-4 9.62 134 11158 184 13.86 248 18.93 436.56 68 8.25 93 9.64 135 i162 188 13.60 250 18.01,Continuation Table 2 7 = time of airflow in seconds; \/F - the factor for use in the r VF oo VFor VP or Wor vt 42-4 6.60 66-4 8.28 93-4 9.67 136 11.66 166 13.64 252 15.87 44 6.63 69 8.31 94 9.70 137 11.70 nT 13.67 254 15194 Mé-e 6.67 69-4 8.34 94-4 9.72 138 11175 82 13.71 256 16.00 45 6.71 70 8137 95 9.75 139 31:79 189 19.75 258 16.06 M54 6175 70-4 9.40 95-4 9.77 140 11183 190 23.78 260 16.12, 466.78 72 8.43 96 9.80 141 11,87 191 19.82 262 16.19 46% 6.82 71-4 0.46 96-4 9.82 142 11192 192 13186 264 16.25, 47 6.86 72 9.49 97 9.85 143 11.96 193 13.89 266 16.32, 47-4 6189 72-4 8.51 97-4 9.87 144 12100 194 13:93 268 16.37 42 6.93 73 8.54 98 9.90 145 12108 195 13.96 270 16.43 49-4 6.96 73-4 49 7.00 74 49-4 7108 Ta 0. 7.07 75 50-4 7.11 75-4 98-4 9.92 146 12.08 196 14.00 272 16.49 99 9.95 147 12,12 197 14.04 274 16.55 99-4 9.97 149 12:37 198 14.07 276 16-61 300 16.00 149 12-21 199 14:11 278 16.67 joo-w10.02 150 12.25 200 14.14 280 16.73Se eB RRR R RR RRR RRR RODE land Plunger Monometer en oee BLAINE AIR PERMEABILITY TEST figure2DETERMINATION OF NORMAL CONSISTENCY OF HYDRAULIC CEMENT SIGNIFICANCE : ‘This test determines the amount of vater required to prepare hydraulic conent pastes for testing. 1. Weights and Weighing Devices - The weights and weighing Gevices shall conform te the requirenents of Specification ASTM ©1005. The weighing device shali be evaluated for precision and | accuracy at a total load of 1,000 g. 2. Glass Graduates - 200 or 250 mi capacity 3. Vicat Apparatus - The vicat apparatus shall consist of a frame A, (Figure 3) bearing a movable rod B, veighing 300 9, one end Cy ! the plunger end, being 10 mm in diameter for a distance of at least 50 mm, and the other end having a removable needle D, 1 mm in diameter and 50 mm in length. The rod B is reversible, and can be held in any desired position by a set screw &, and has an adjustable indicator P which moves over s scale (graduated in fillinetzes) attached to the frame A. The paste is held in a rigid conical ring G, resting on a plane fon-absorptive base plate H about 100 mm?. The rod 8 shall be made of stainless Steel having a hardness of not less than 35 HRC, and shall be straight with the plunger end which is perpendicular to the rod axis. The ring shall be made of a noncorreding, nonabsorbent material, and shall have an inside dianeter of 70 mm at the base and 60m at the top, and a height of 40 mm. PROCEDURE 2. Mixed a 650 grams of cement with a measured quantity of clean Water following the procedure of mixing of Hydraulic Cement Pastes and Mortars of Plastic Consistency, as follows a) Place all mixing water in the bowl. b) Add cement to the water and allow 30 s for the absorption of the water. ©) Start mixer and mix at slow speed (140 + 5 rpm) for 30 @) Stop the mixer for 15 s and during this tame scrape down into the batch any paste that may have collected on the sides of the bowl. ©) Start the mixer at medium speed (285 + 10 rpm) and mix for 1 2. Quickly form the cement paste into a ball and toss six times from one hand to the other maintaining the distance between the hands about 150 mn apart. 2 EePress the ball into the larger end of the conical ring, filling the ring with paste, completely. Renove the excess at the larges fend by @ single movement of the palm of the hand) Place the ring on @ base plate resting on larger end. Slice off the excess paste at the smaller end by a sincle sbligae Stree of a sharp-edge trowel. ‘Take care not to compress the “enote during cutting or snocthing excess paste. Center the paste confined in the ring, resting on the plate, under the rod of the vicat apparatus, with the end’ df the Plunger in contact with the surface of the paste Set the moving indicator to the upper zero back of the scale, or take an initial reading and release the rod inmediately which Rust not exceed 30 seconds after completion of mixiag. ‘the apparatus shall be free of vibration during the test. she paste shall be of normal consistency when the rod settles to's point 10 + i mm below the original surface in 30 seconds after being relgased 7. Make trial pastes with varying percentages of water until the normal consistency is obtained. ‘CALCULATION : Calculate the amount of water required for normal consistency to the Rearest 0.1 percent and report it to the nearest 0.5 percent of the weight of the dry cement. volume of water required (cn) me WE. of Cement sample (650 9) 3 meee eee eeeVICAT APPARATUS figure 3DETERMINATION OF TIME OF SETTING OF HYDRAULIC CEMENT BY 1 (GILLMORE NEEDLE SIONIFICANCE AND USE: The purpose of this test method is to establish whether a cement eouplies with a specification limit on setting tine. The time of setting is affected not only by the percentage and temperature of the water used, and the amount of kneading the paste received, but also by the tenperature and Genidity of the air. ‘APPARATUS : i. Trowel, having 2 steal blade 100 to 150 mm (4 to 6 in.) in Length, with a straight edge. 1 A A 2. Mixer, Bowl, Paddle, and Scraper; 3. Glass Graduates, Scales and Weights, conforming to the requirements wf Specification ASTM c i005 5. Glass Plates, flat, 102 mm (4 in.) square. 6. Gilmore Needles, conforming to the following requirements: 6.1 The initial setting-time needle shall have a weight of 313.44 0.5 @ (0.25040.001 1b) and a tip diameter of 2.1245.05 mm (0.08430.002 in.) The final setting time needle shall have a weight of 493.640.5 g (1.00020.001 1b) and @ tip diameter of 1.06 40.05 mm (0.04240.002 in.) 6.3 The needle tips shall be cylindrical for a distance of 4,840.5 nm (0.189¢0.020 in.} ‘The needle ends shall be piane and at right angles to the axis of the rod and shall be maintained in a clean condition. The Gilmore needies should preferably be mounted as shovn in Figure 4. 1. Preparation of Cement vaste - Mix 650 g of cement with the percentage of rising water required for normal consistency Following the mixing procedure for cement pastes: fielinenlin eee, 2. Molding Test Specimen - From the cement paste prepared as = described in i, make a pat approximately 76 mm (2 in.) in diameter and approximately 13 mm (0.8 in.) in thickness at the center with a fiat top and tapering to a thin edge (see Figure = 4) on & clean glass plate. In molding the pat, flatten the Genent paste fizst on the glass and then form the pat by drawing the trowel from the cuter edge toward the center, then = flattening the top. After making, place the pat in the moist 15eabinet or moist room and allow it to remain there except when the determinations of tine of setting are being made Time of Setting Determination - In determining the tine of setting, hold the needles in s vertical position and apply Lightly’ to the surface of the pat. consider the cement paste to have acquired its initial set when the pat will beat, without, appreciable indentation, the initial ‘Gillmore needle, The Gifference, in minutes, ‘between the time of contact of coment and mixing water and the time the cenent paste acquires its initial set is the initial setting tine. Consider the cement Paste to have acquired its final set when the pat vill bear, without appreciable indentation, the final Gillnore needle. The difterence, in minutes, between the time of contact of cement and mixing water and the tine the cement paste acquires its ‘Tho report shall show the time of setting as follows Initial Tine of Setting, Gillnore ---~- min. Final Time of Setting, Gilimore eaeBnet DETAL OF nezELe ps seen meat ans ssemariegt Sera Brine Fate oe wees GILLMORE APPARATUS AND TEST SPECIMEN figure 4 veAPPARATUS PROCEDURE, 1 ‘DETEAMINATION OF TIME SETTING OF HYDRAULIC CEMENT By VICAT NEEDLE scales and Weights Graduated cylinder, 200 or 250 ml capacity Vicat apparatus shal consist of a Frame, A, see Fig. 5, bearing a movable rod, By weighing 300 9, one end, c, the plunger end, being 10 mm Toa iactor for a distance of at least 50 am and other end faving a removable steel needle, D, 1 mm in dianeter and 50 mm nevig gtho the rod B is reversible and can be held in any ateived position by a set screw, =, and has an adjustable geaitetor F, which moves over a scale attached to the frame, specertre ia held in a conical ring, G, resting on a glass see ee Re bout 100 mn square. The ting shall be made of Pencerroding, nenabsorbing material, and shall have an inside ceeeeter of 70 mm at the base and 60 nm at the top and a height SE"fo mn. The vicat apparatus shall conform to AASHTO T 131 Preparation of Cement Paste Mix 650 9 of cement with the percentage required for normal consistency following the procedure of mixing of Hydraulic Eoment Pastes and Mortars of Plastic Consistency. Molding of Test specimen a) Quickly form a cement paste into = ball and toss six (6) Quick Gn one hand to the other maintaining the distance Between the hands about 152 nm epart. b) Press the’ ball into the large end of the conical ring, Piling the ving with paste completely. Renove the excess Eine isrger end by a single movenent of the palm of the hand, c) Place the ring on its larger end on a glass plate. slice Place she wxcess paste at the smaller end by a single Sblique stroke of a sharp-edged trovel, Take care not to oblique Stine paste during cutting or smoothing excess paste. 4) amediately after molding, place the speciman in the moist ‘Meee or moist room with a temperature of 23°C (73.4°F) si85ec tary); and allew it to remain there except vhen Bee Scions ‘of tine of setting are being made. The seerren Ghai renain in the conicel mold, supported Py eRetGless plate, H, throughout the test period. aeEa Tine of setting Determination 2) Allow the specimen to remain in the moist cabinet or room for 30 min after molding without being disrareeg” Determine the penetration of the 1 mm needle at this tine and every 18 min thereatter until a penetration of 25 nn, or less is obtained b) For the Penetration test, lover the needle D of the rod 8 until it ‘rests on the surface of the cement peeves Tighten the set screw, E, and set the indicator, F, St the Neper end of the scale, or take an initial ‘reading Release the rod quickly by releasing the set screw, a, eta alloy the needle to settle for 30 s, then take the’ reading fo determine the penetration. No penetration test shall be made Closer than 1/4 in. (6.4 mn) from any previone Penetration and nor shall be made closer than 3/8 fn to's fm) from the inside of the mold. ©) Record the results of all penetration tests and, by interpolation determine the tine when a penctration of 2 mm is obtained which is the initial setting time. 9) At the time the needle does not sink visible into the Paste, it is considered to be the final setting time, asae eReR RRR ERR RR RRR aaa SOUNDNESS DETERMINATION OF PORTLAND CEMENT BY AUTOCLAVE EXPANSION SIGNIFICANCE : ‘The autoclave expansion test provides an index of potential delayed expansion caused by the hydration of Calcium Oxide (C20) or Magnesium Oxide (Qigo) oF both. APPARATUS = 1 2 6 Scales and weights cylinder, graduated, 200 mi capacity Molds, 25.4 x 25.4 rm cross section Trowel - having a straight-edge steel blade 4 to 6 in. (100 to 180 mm) in Length. Autoclave apparatus, conforming to the requirement of ASTM Cc 151-749 Length comparator, for measuring length change of specimen. PROCEDURE + 1 Prepare a cenent paste of normal consistency, consisting of 650 J of cement and sufficient amount of water, Mix this both in accordance with procedure for Mechanical Mixing of Hydraulic Cenent Pastes and Mortars of Plastic Consistency. Immediately following the completion of the mixing, place the paste in the molds in two approximately equal layers, each layer being compacted with the thumb or forefingers by pressing the Paste into the corners, around the gage studs, and along the surface of the mold until a homogeneous specimen is obtained, Compact ths top layer, cut eff the paste flush with the top of the mold and snosthen the surface with a few strokes of the Exowel. Daring the operations of mixing and molding, protect the hands with rubber gloves Store specimens in the molds in the moist room for at least 20 hours. If remove from the molds before 24 hour, they shell be Kept in the moist room until time of test At 24 nours + 20 minutes after molding, remove the specimens from the moist atmosphere and immediately measure the length, Place the specimens in the autoclave with enough water at an initial temperature of 68 to 82°F (20 to 28°C) to maintain an stmosphere of saturated steam vapor during the entire test. Jo permit air to escape from the autoclave during the early portion of the heating period, leave the vent valve open untit aasteam begins to escape. Close the valve and raise the tonperature of the autoclave at a rate that will bring the gage pressure of the steam to 295 psi (2 Mea) in 45 to 75 min from fhe tine the heat is turned on Maintair the 295410 psi (240.07 MPa) pressure for 3 h. At the end of 3h period shut off the heat supply and cool the Sutoclave. surface dry the specimens and measure the length. ‘CALCULATION: calculate the difference in length of the test specimens before and after autoclaving as percent of the affective gage length and report to the Rearest 0.01 percent, Report the percentage of increase in length as the dutoclave expansion. Indicate @ decrease in length by a minus sign prefixed to the percent value 2DETERMINATION OF AIR CONTENT OF HYDRAULIC CEMENT SIGNIFICANCE The purpose of this test 1s to determine whether or not the hydraulic cement under test meets the air-entraining ae Eequirements of the applicable hydreuii fest is being made, non-airventraining ic ecment specification for which the Plow Table, Flow Mold, and Caliper - conforming te the Fequirements of Specification M 182 Measure -A cylindrical measure having an inside diameter of 341/16 in. (76.2 4 1.6 mm) and depth (approximately 3 19/32 in 1 mm)) adjusted by standardization with water to contain 400 4 imi at 23¢17°C (73.4 + 3°F) Mixer, Bowl and Paddle Straightedge - A steel straightedge not less than 4 in, (102 mm) dong and not less than 1/16 in. (1.6 mm) nor more than i/3 tn (3.2 mm) in thickness. 5. Spatula spatula with a metal blade 6 in. (152 am) in length and 1/2 in. (13 mm) in width, with straight edges and a woolen handle. 6, Weights and Weighing Devices - the weighing device shall be evaluated for precision and accuracy at a total load of 7 to 7. Glass Graduates - Glass graduates of 250-ml capacity, vith graduations at 2-ml intervals, for measuring the mixing ‘waver, made to deliver the indicated volume at 68°F (20°C) Tamper - made of nonabsorptive, nenabrasive, nonbrittle material in. (16 mm) and a length of 6 in. (152 mm) 31, spoon = A metal restaurant serving spoon at least 9 in. {approximately 230 mn) in length and with a bowl approximately 4 ine (100 mm) in length. 12. Standard Sand - patural silica , 4 10. Tepping Stick ~ made of hard wood and having a diameter of 5/8PROCEDURE Prepare the standard mortar ‘for test using the proportion 350 of coment to 1400 g of standard sand and sufticient water, te Give a flow between'ay 1/2 #7 1/2 percent Mix the mortar in accordance with the following manner: a) Place all the mixing water in the bowl. b) Add cement to the water then start the mixer and mix at the low speed’ (40 + 5 rpm) for 30 seconds. ©) Add the entire quantity of sand slovly over a 30 s period, while mixing at slow speed 4) Stop the mixer, change to medium speed (285 + 10 zpm) and mix for 30 seconds. 2) Stop the mixer and let the mortar stand for 90 seconds. During the first 15 seconds of this interval, quickly scrape down into batch any mortar that may have ‘collected on the side of the bowl, then for the remainder of this interval, cover the bowl ith the lid £) Finish by mixing for 60 = at medium speed (285 + 10 pm) Determine the flow of the mix in the following manne: a) Using @ spoon, place a layer of mortar about 25 mm thick in the mold and tamp 20 times with the tamper. The tamping pressure shall be Just sufficient to. insure uniforn Filling of the mold. Then fill the mold with mortar and tanp 2s specified for the first layer. Then cut off the mortar to a plane surface. Flush with the top of the mold Using straignt edge of the trovel. One minute after completing the mixing operation, remove the mold and Inmediately, drop the flow table through a height of 12.7 mi 10 times in @ s. The flow is the Yesulting increase in average dianeter of the mortar mass, measured on at least four diameters, expressed as percentage of the original Gianeter. Make trial mortars with varying percentages of Water until the specific flow is obtained. Make each trial with fresh mortar. b) Weight per 400 ml of Mortar: hen the ideal quantity of vater has been found that produces a flow of @7-1/2 + 7-1/2 percent, inmediately Sctermine ‘the weight per 400 ml of mortar, using the mortar remaining in the mixing bovl after the flow has been determined. In the determination of the weight per 400 mi, do not Use the portion of the mortar used in the flow determination, Using the spoon, fill the 400-m) measure with the mortar, in three (3) equal layer, tamping ‘ach layer 20 times vith the tamper around the inner Surface of the measure, Each layer is tamped in one 2aR eR eR RRO RERERERERERE EERE ‘CALCULATION complete revolution with only sufficient pressure to adequately fill the measure and eliminate the voids within the mortar. The position of the tamper shall be that: the broad side of ‘the tamper always coincides with the direction of the radius and is perpendicular to the snner surface of the measure. After the measure has bean filled and tanped, tap the sides of the measure lightly with the Sides of the tapping stick once each at five different points at approximately equal spacing around the outside Sf the measure, in order to. preclude entrapment of extraneous sir. Then cut off the mortar toa. plane Surface. Flush vith the top of the measure by drawing the Straight edge with a sawing motion across the top of the Measure, making two (2) passes over the entire surface, the second pass being made at right angles to the first Then weigh the measure filled with mortar. subtract the weight of the container, and recard the weight of the mortar in grams. ‘The formula is applicable only on portland cement having a specific gravity of 3-15, ether than 2.15 substitute appropriate value for its Specific gravity. Aix Content, volume & where: (282.7 +P) 100 = Wo manennnnnnene [2000 + 4P) W = weight of 400 mi of mortar, gy and e percentage of mixing water, based on weight of coment used 25DETERMINATION OF COMPRESSIVE STRENGTH OF HYDRAULIC CEMENT MORTARS (USING 50 mm CUBE SPECIMENS) SIONEProaNcE : This method used to determine the compressive strength of hydraulic cement that will be used to determine compliance with specification’. APPARATUS : Weights and Weighing Devices, shall conform to the requirements of “ASTM C 1005 the weighing device shall be ‘evaluated for precision and bias at a total load of 2,000 g. Glass Graduated, of suitable capacities (preferably large enough to measure the mixing water ina single operation) to deliver the indicated volume at 68°F (20°C). Specimen molds for the 50 mm cube specimens shall be tight fitting and shall have not more than thres (3) cube compartments and shall be separable into not more than to (2) parts. The mold shall be made of hard metal not attacked by cement mortar. Mixer, Bowl and Paddle, an electrically driven mechanical mixer of the type equipped with paddle and mixing bowl. Flow table and flow mold, conforming to the requirement of ASTH © 230/AasHTO 7-106. Tamper - The tamping face shall be flat and at right angles to the length of the tamper with a cross section of 13 x 25 nm and a Length of about 120'to 150 mm Trowel ~ with a steel blade 100 to 150 mn length, straight edge Testing Machine - either the hydraulic or the screv type, with sufficient opening between the upper bearing surface and the lower bearing surface of the machine to permit the use of verifying apparatus. PROCEDURE : Prepare the standard mortar to be used for the test using the Proportion one (1) part cement to 2.75 parts of graded standard sand by weight. The amount of mixing water shall be such as to Produce a flow of 110¢ as determined in accordance vith Procedure number 2, ‘The quantities of materials to be used at one tine in the batch of mortar for six or nine test specimens shall be as follows: 26se eee RR ER ERO! bal ~~ ehh Number of specimens: cement, 500 sand) g 1373 2035 Water, ml Portland (0.485) 242 358 Aie-entraining Portland (0.460) 230 240 other (to flow of 11045) =~ - ‘The materials shall be mechanically mix in the following manner: a) Place all the mixing water in the bowl, b) Add coment to the water and mix at the slow speed (140 + 5 zpm) fer 30 seconds. ©) Add the quantity of sand slowly over a 30 seconds period, while mixing at a slow speed. @) Stop mixer, change the speed to (285 + 10 xpm), and mix for 30 seconds. ©) stop the mixer and let the mortar stand for 1-1/2 minute During the 15 seconds of this interval, quickly scrape down into the batch any mortar that may have collected on the side of the bowl, then for the remainder of this interval, cover the bowl with the lid Finish the mixing for 1 minute at the speed (285 + 10pm) 9) In any case requiring a remixing interval, any mortar adhering to the side of the bowl shali be quickly scraped down into the batch with the scraper prior to remixing. To determine the flow, place a layer of the prepared mortar about 25 mm in thickness in the flow mold and tamp 20 tines with the tamper. The tamping pressure shall be just sufficient to insure uniform filling of the mold. Then fili the mold with mortar and tamp as specified for the first layer. cut off the mortar to plane surface, flush with the top of the mold using straight edge of the trowel. One (1) minute after completing the mixing operation, remove the mold and immediately, drep the flow table 25 tines through a height of 12.7 mn in 15 seconds. ‘the flow is the resulting increase in average dianeter of the base of ‘the mortar mass, measured on at least’ four dianeters, expressed as percentage of the original dianeter. Make trial mortars with varying amount of water until the specified flow is obtained. Make each trial vith fresh mortar: aImmediately after completion of the flow test, quickly scrape down into the batch the mortar that may have collected on the side of the bowl and then remix the entire batch 15 seconds. Start molding the specimens within the elapsed time of not more than 2 minutes and 30 seconds after completion of the original mixing of the mortar batch. Place a layer of mortar sbout 25.4 mm in thickness in all of the cube compartment. Tamp the mortar in each cube conpartnents 32 times in about 10 seconds in 4 rounds, each round to be at right angles to the other and consisting of 8 adjoining strokes. The tanping pressure shall be Just sufficient to insure uniform filling of the molds. The 4 Founds of tamping with 32 strokes of the mortar shall be completed in one cube before going to the next. When the tamping of the first layer in all of the cube compartments is completed, fill the compartment. with the remaining mortar and then tanp as specified for the first Layer. During tamping of the second layer, bring in the mortar forced Sut onto the tops of the molds after each round of tamping by means of the gloved fingers and tanper upon completion of each Found and before starting the next round of tamping. On completion of the tamping, the tops of all cubes should extend slightly above the tops of ‘the molds. Bring in the mortar that has Been forced out onto the tops of the molds with a trowel and smooth off the cubes by drawing the flat side of the trowel once across the top of each cube at right angle to the length of the mold. Cut off the mortar to a plane surface flush with the top of the mold by drawing the straight edge of the trowel with a saving motion over the length of the mold. Immediately upon completion of the molding operation, place the test specimens in the moist closet or moist room about 20 to 24 hours with their upper surfaces exposed to the moist air but protected from dripping water. After 24 hours, remove specimens from the molds, and then immerse in saturated lime water until the tine of test, except those specimens that are to be tested after 24 hours, : Test the specimens innediately after their removal from the moist closet in the case of 2é-hour specimens, and from storage Water in case of all other specimens. All test specimens for a Given test age shall be broken within the permissible tolerance Prescribed as follows: Test age Permissible Tolerance aan fan 3 days Fin 7 days Fan 28 days Fizh 284. Balance Analytical - shall have @ sensitivity of 0.0001 g. 2, desiccator 3. Grucibles, platinum, 15 to 30 mi capacity 4, Mafle furnace, capable of continuous operation up to (1200°C) 2192°F and should have an indicating pyroneter accurate to + (25 sc) 7 PROCEDURE 1. Weigh 1 9 of the sample in a platinum crucible and ignite ‘the Crucible and its contents to constant weight in a muffle furnace 2. Allow a minimum of 15 min. for the heating period. 3. Cool te room temperature in a dessicator and weigh CALCULATION Calculate the percentage of loss on ignition to the nearest 0.1 by multiplying the loss in weight in grams by 100 We, of Sample _ Wt. of Sample before ignition” After ignition § uoss on Ignition = = sas X 100, Weight of SampleAPPARATUS a) by 2) 4) ° t) 0 [PROCEDURE DETERMINATION OF INSOLUBLE RESIDUE Balance Analytical, shall have a sensitivity of 0.0001 g. Gjesswares such 2s flasks beakers, graduated cylinder, should be of precision grade or bette £ a Desiceator Filter Paper Crucibles, platinum, or porcelein 15 to 30 mi capacity Muftle furnace, capable of continuous operation up to (120%) 2192°F and should have an indicating pyrometer accurate to + 77°F (25°C) Reagents, such as : Sodium Hydroxide Solution (10 g NaOH/1iter) Hydrochloric Acid - sp. gr. 1.19 Methyl Red Indicator - 2 g/liter with 95 § ethyl alcoho? 76 1 gram of the sample, add 25 ml of cold water. Disperse the cement in the ater and vhile svirling the mixture, quickly add 5 mi of Hel. Dilute the solution to 50 ml with hot water nearly boiling and digest the mixture. Filter the solution through mediun-texture paper into a flask, wash the flask, paper anu residue thoroughly with hot water, and Eeserve the filtrate for the sulfur trioxide determination, if desired. : Transfer the filter paper and contents to the original beaker, add 100 ml of hot (near boiling) NaOH solution (10 g/liter) and digest. Acidity the solution with Wel using methyl red as the indicator and filter again through mediun-textured paper. Wash the residue at least 14 times with hot water making certain 0 wash the entire filter paper and contents during each washing Ignite the residue in a weighed platinum crucible at 1652°F to 18329F (800 to 1000%C}, cool in a desiccator and veagh CALCULATION aii itr rth herr rrr ree Galculate the percentage of Insoluble Residue to the nearest 0.01 by ‘tiplying the weight in grams of the residue (corrected for the blank) by aDETERMINATION OF SULFUR TRIOXIDE CONTENT APPARATUS 2) Balance Analytical, shall have 2 sensitivity 0.0001 g with dD) Glassyares, such as, flasks, beakers, graduated cylinder, Porcelein disk should be of peécision gude Sr patter, “YReE ©) desiccator 4) Filter paper fe) Crucibles, platinum, or porcelein 15 to 30 ml capacity £) Muffle furnace, capable of continuous operation up to 2192°F (3200°c) and should have an indication pyrometer accurate to TIPE (25°C). 9) Reagents, such as : Bariun Chloride (BaCl) - 100 g/liter 1. 70.2 g of the sample add 25 mi of cold water and while the mixture is stirred vigorously, add 5 mi of HCL. If necessary, heat the solution and grind the material with the flattened end of a glass rod until it is evident that decomposition of the cement is complete: 2. pilute the solution to 50 ml and digest for 15 min. at @ temperature just below oiling 3. Filter through a medium textured paper and wash the residue thoroughly with hot water 4, itute the filerate obtained after removing the insoluble residue £2 250 ml and heat to boiling. Add 10 ml of hot barium chioride, BaClz (100 g/liter) and continue the boiling until the | precipitate is well formed. Digest the solution at a temperature Below boiling. Let the solution stand overnight 5. Filter the precipitate, vash with hot water, place the paper and contents ina weighed platinum crucible and char and consume the | paper without inflaning. Ignite to 1472°F up to 1652°F (800 to 900°C), cool in a desiccator, and weigh cateutarron : | Calculate the percentage of $03 to the nearest 0.01 as follows: | we 304 503 percent = ~ s 2 where w= grams of Barium Sulfate (82504), and 34.3 = molecular ratio of 503 to BaS0,’ (0.343) multiplied x 100DETERMINATION OF MAGNESIUM OXIDE CONTENT: a) Balance Analytical, shail have a sensitivity of 0.0001 g. b) Glasswares, such as flasks, beakers, graduated cylinders, porcelein disk, ete c) desiccator ) Filter paper fe) Ceucibles, platinum, or porcelein 15 to 30 mi capacity #) Muffle furnace, capable of continuous operation up to 21929 (2200°c) and should have an indication pyrometer accurate to 77°F (288C) ¢) Reagents Ammonium Nitrate Wash Solution - Dissolve 100 9 of Ammonium Nitrate (NHq-NO3) in water, and 200 ml of Ni4OH, dilute to 1 liter, and store in a plastic bottle. 2, Ammonium Phosphate, Dibasic (100 g/liter), (Niy)2HPO, 3. Ammonium Oxalate solution = 50 g/liter 4.0 HEL ~ sp. gr. = 1.9 NHgOH - sp. ge. = 0.90 6. Methyl red ~ 2 g/liter of 958 ethy1 alcohol PROCEDURE a 1, Weigh 0.50 g sample and place it to a 400-mi beaker 2, Add 10 mi of cold water (disperse the sample in a swirling motion using a flattened end of = glass rod). 3. Add to 10 ml HCL (digest with the aid of gentle heat and agitation untit decomposition is complete). 4. Evaporate the solution to disperse on a steam bath (or on a hot. Plate or stove with a low flane) until there is no gelatinous appearance 5. Then after drying, treat it with 10 ml HCL, wait at least 2 min., and then add an equal amount of water (10 mii. Digest for 10 min. on the steam bath or hot plate 3Filter the solution through a medium textured paper and vash the residue with hot water. Discard the residue (Si02) 8. To the filtrate (at east have a volune of about 150-175 m), add a few drops of methyl red indicator (one or two drops) and heat to boiling (red color) 9. Then treat the solution with Miigo# until the precipitate formed (brown precipitate) and the color of the solution becomes yellow. 10. eat the solution containing the precipitate to boiling and boil for $0 to 60 seconds 11, Allow the precipitate to settle (not more than 5 min) and then filter. 12. Mash the precipitate with hot water, discard residue (HoH Group) 12. To the filtrate (at least have a volume of about 200-225 ml), add 30 ml of warm Ammonium Oxalate soluticn. 14. Heat the solution to 70 te 80°C. 15. Allow the solution to stand for 6045 mins. then filter the Solution, wash the precipitate with hot vater, discard the Fesidue (Ca0) 16. To the filtrate (at least have 2 volume of 225-250 ml), add 10 mi. (Mig) gHPOq solution. Stir the solution until the crystalling magnesium anicniun precitate begins to form. 17. Set the solution aside for at least 6 hrs 18. Then filter, and wash the residue with hot water with anmonia wash solution, discard the filtrate, to the residue place it in 8 crucible and then ignite @ 100°C in a furnace, 19. Cool and then weigh as magnesium pyrophosphate (€g2207) CALCULATION calculate e percentage of Ngo to the nearest 0.1 as follows: Ngo = Wx 72.4 Mo = grams of MggP207, and molecular ratio of 2 tg0 to MgzP207 (0.362) divided by the weight of sample used (0.5 9) fand maltiplied by 200 a4