IC-NRLF SB 7b IbE GIFT OF Standard Specifications and Tests for Portland Cement of the American Society for Testing Materials Affiliated with the International Association for Testing Materials Philadelphia, Pa. These specifications are the result of several years' work of a special committee representing a United States Government Departmental Committee, the Board of Direction of the American Society of Civil Engineers, and Committee C-l on Cement of the American Society for Testing Materials, in cooperation with Committee C-l. "Concrete for Permanence" Reprinted by Portland Cement Association ATLANTA Hurt Building INDIANAPOLIS Merchants Bank Building PABKERSBUBG, W. VA. Union Trust Building DECEMBER. 1916 Offices at CHICAGO DALLAS 111 W. Washington Street Southwestern Life Building KANSAS CITY NEW YORK Commerce Building PITTSBURGH Farmers Bank Building 101 Park Avenue SAN FRANCISCO 116 New Montgomery Street Authorized Reprint from the Copyrighted A.S.T.M. STANDARDS (1916) AMERICAN SOCIETY FOB TESTING MATERIALS, PHILADELPHIA, PA. STANDARD SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 1 Serial Designation: C -17. Definition. 1. Portland cement is the product obtained by finely pul- verizing clinker produced by calcining to incipient fusion an intimate and properly proportioned mixture of argillaceous and calcareous materials, with no additions subsequent to calcina- tion excepting water and calcined or uncalcined gypsum. I. CHEMICAL PROPERTIES. Chemical 2. The following limits shall not be exceeded: Limits. Loss on ignition, per cent 4 . 00 Insoluble residue, per cent . 85 Sulfuric anhydride (SO 3 ), per cent 2 . 00 Magnesia (MgO), per cent 5 . 00 II. PHYSICAL PROPERTIES. Specific Gravity. x 3. The specific gravity of cement shall be not less than 3.10 (3.07 for white Portland cement). Should the test of cement as received fall below this requirement a second test may be made upon an ignited sample. The specific gravity test will not be made unless specifically ordered. Fineness. 4. The residue on a standard No. 200 sieve shall not exceed 22 per cent by weight. Soundness. 5. A pat of neat cement shall remain firm and hard, and show no signs of distortion, cracking, checking, or disintegration in the steam test for soundness. Time of Setting. 6. The cement shall not develop initial set in less than 45 minutes when the Vicat needle is used or 60 minutes when the Gillmore needle is used. Final set shall be attained within 10 hours. Tensile strength. 7. The average tensile strength in pounds per square inch of not less than three standard mortar briquettes (see Section 5 1) 1 These specifications and tests were adopted by letter ballot of the Society on September 1, 1916, with the understanding that they will not become effective till January 1, 1917. (2) SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 3 composed of one part cement and three parts standard sand, by weight, shall be equal to or higher than the following: Age at Test, days. Storage of Briquettes. Tensile Strength. Ib. per sq. in. 7 200 28 300 8. The average tensile strength of standard mortar at 28 days shall be higher than the strength at 7 days. III. PACKAGES, MARKING AND STORAGE. 9. The cement shall be delivered in suitable bags or barrels Packages and with the brand and name of the manufacturer plainly marked thereon, unless shipped in bulk. A bag shall contain 94 Ib. net. A barrel shall contain 376 Ib. net. 10. The cement shall be stored in such a manner as to per- storage, mit easy access for proper inspection and identification of each shipment, and in a suitable weather-tight building which will protect the cement from dampness. IV. INSPECTION. 11. Every facility shall be provided the purchaser for care- inspection, ful sampling and inspection at either the mill or at the site of the work, as may be specified by the purchaser. At least 10 days from the time of sampling shall be allowed for the com- pletion of the 7-day test, and at least 31 days shall be allowed for the completion of the 28-day test. The cement shall be tested in accordance with the methods hereinafter prescribed. The 28-day test shall be waived only when specifically so ordered. V. REJECTION. 12. The cement may be rejected if it fails to meet any of Rejection, the requirements of these specifications. 13. Cement shall not be rejected on account of failure to meet the fineness requirement if upon retest after drying at 100 C. for one hour it meets this requirement. 14. Cement failing to meet the test for soundness in steam* 347146 SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. Number of Samples. Method of Sampling. Treatment of Sample. may be accepted if it passes a retest using a new sample at any time within 28 days thereafter. 15. Packages varying more than 5 per cent from the speci- fied weight may be rejected; and if the average weight of pack- ages in any shipment, as shown by weighing 50 packages taken at random, is less than that specified, the entire shipment may be rejected. TESTS. VI. SAMPLING. 16. Tests may be made on individual or composite samples as may be ordered. Each test sample should weigh at least 8lb. 17. (a) Individual Sample. If sampled in cars one test sample shall be taken from each 50 bbl. or fraction thereof. If sampled in bins one sample shall be taken from each 100 bbl. (b) Composite Sample. If sampled in cars one sample shall be taken from one sack in each 40 sacks (or 1 bbl. in each 10 bbl.) and combined to form one test sample. If sampled in bins or warehouses one test sample shall represent not more than 200 bbl. 18. Cement may be sampled at the mill by any of the following methods that may be practicable, as ordered: , (a) From the Conveyor Delivering to the Bin. At least 8 Ib. of cement shall be taken from approximately each 100 bbl. passing over the conveyor. (b) From Filled Bins by Means of Proper Sampling Tubes. Tubes inserted vertically may be used for sampling cement to a maximum depth of 10 ft. Tubes inserted horizontally may be used where the construction of the bin permits. Samples shall be taken from points well distributed over the face of the bin. (c) From Filled Bins at Points of Discharge. Sufficient cement shall be drawn from the discharge openings to obtain samples representative of the cement contained in the bin, as determined by the appearance at the discharge openings of indicators placed on the surface of the cement directly above these openings before drawing of the cement is started. 19. Samples preferably shall be shipped and stored in air- tight containers. Samples shall be passed through a sieve SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 5 having 20 meshes per linear inch in order to thoroughly mix the sample, break up lumps and remove foreign materials. VII. CHEMICAL ANALYSIS. Loss ON IGNITION. 20. One gram of cement shall be heated in a weighed cov- Method, ered platinum crucible, of 20 to 25-cc. capacity, as follows, using either method (a) or (b) as ordered: (a) The crucible shall be placed in a hole in an asbestos board, clamped horizontally so that about three-fifths of the crucible projects below, and blasted at a full red heat for 15 minutes with an inclined flame; the loss in weight shall be checked by a second blasting for 5 minutes. Care shall be taken to wipe off particles of asbestos that may adhere to the crucible when withdrawn from the hole in the board. Greater neatness and shortening of the time of heating are secured by making a hole to fit the crucible in a circular disk of sheet plat- inum and placing this disk over a somewhat larger hole in an asbestos board. (b) The crucible shall be placed in a muffle at any tempera- ture between 900 and 1000 C. for 15 minutes and the loss in weight shall be checked by a second heating for 5 minutes. 21. A permissible variation of 0.25 will be allowed, and all Permissible results in excess of the specified limit but within this permissible Variation - variation shall be reported as 4 per cent. V^ INSOLUBLE RESIDUE. 22. To a 1-g. sample of cement shall be added 10 cc. of Method, water and 5 cc. of concentrated hydrochloric acid; the liquid shall be warmed until effervescence ceases. The solution shall be diluted to 50 cc. and digested on a steam bath or hot plate until it is evident that decomposition of. the cement is complete. The residue shall be filtered, washed with cold water, and the filter paper and contents digested in about 30 cc. of a 5-per-cent solution of sodium carbonate, the liquid being held at a temper- ature just short of boiling for 15 minutes. The remaining residue shall be filtered, washed with cold water, then with a few drops of hot hydrochloric acid, 1 : 9, and finally with hot 6 SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. water, and then ignited at a red heat and weighed as the insoluble residue. Permissible 23. A permissible variation of 0.15 will be allowed, and all on " results in excess of the specified limit but within this permissible variation shall be reported as 0.85 per cent. SULFURIC ANHYDRIDE. Method. 24. One gram of the cement shall be dissolved in 5 cc. of concentrated hydrochloric acid diluted with 5 cc. of water, with gentle warming; when solution is complete 40 cc. of water shall be added, the solution filtered, and the residue washed thoroughly with water. The solution shall be diluted to 250 cc., heated to boiling and 10 cc. of a hot 10-per-cent solution of barium chloride shall be added slowly, drop by drop, from a pipette and the boiling continued until the precipitate is well formed. The solution shall be digested on the steam bath until the precipitate has settled. The precipitate shall be filtered, washed, and the paper and contents placed in a weighed plat- t inum crucible and the paper slowly charred and consumed without flaming. The barium sulfate shall then be ignited and weighed. The weight obtained multiplied by 34.3 gives the percentage of sulfuric anhydride. The acid filtrate obtained in the determination of the insoluble residue may be used for the estimation of sulfuric anhydride instead of using a separate sample. Permissible 25. A permissible variation of 0.10 will be allowed, and all Variation. resu it s in excess of the specified limit but within this permissible variation shall be reported as 2.00 per cent. MAGNESIA. Method. 26. To 0.5 g. of the cement in an evaporating dish shall be added 10 cc. of water to prevent lumping and then 10 cc. of concentrated hydrochloric acid. The liquid shall be gently ! heated and agitated until attack is complete. The solution shall then be evaporated to complete dryness on a steam or water bath. To hasten dehydration the residue may be heated to 150 or even 200 C. for one-half to one hour. The residue shall be treated with 10 cc. of concentrated hydrochloric acid diluted with an equal amount of water. The dish shall be SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 7 covered and the solution digested for ten minutes on a steam bath or water bath. The diluted solution shall be filtered and the separated silica washed thoroughly with water. 1 Five cubic centimeters of concentrated hydrochloric acid and sufficient bromine water to precipitate any manganese which may be present, shall be added to the filtrate (about 250 cc.). This shall be made alkaline with ammonium hydroxide, boiled until there is but a faint odor of ammonia, and the precipitated iron and aluminum hydroxides, after settling, shall be washed with hot water, once by decantation and slightly on the filter. Set- ting aside the filtrate, the precipitate shall be transferred by a jet of hot water to the precipitating vessel and dissolved in 10 cc. of hot hydrochloric acid. The paper shall be extracted with acid, the solution and washings being added to the main solution. The aluminum and iron shall then be reprecipitated at boiling heat by ammonium hydroxide and bromine water in a volume of about 100 cc., and the second precipitate shall be collected and washed on the filter used in the first instance if this is still intact. To the combined filtrates from the hydrox- ides of iron and aluminum, reduced in volume if need be, 1 cc. of ammonium hydroxide shall be added, the solution brought to boiling, 25 cc. of a saturated solution of boiling ammonium oxalate added, and the boiling continued until the precipitated calcium oxalate has assumed a well-defined granular form. The precipitate after one hour shall be filtered and washed, then with the filter shall be placed wet in a platinum crucible, and the paper burned off over a small flame of a Bunsen burner; after ignition it shall be redissolved in hydrochloric acid and the solution diluted to 100 cc. Ammonia shall be added in slight excess, and the liquid boiled. The lime shall then be reprecipi- tated by ammonium oxalate, allowed to stand until settled, filtered and washed. The combined filtrates from the calcium precipitates shall be acidified with hydrochloric acid, concen- trated on the steam bath to about 150 cc., and made slightly alkaline with ammonium hydroxide, boiled and filtered (to remove a little aluminum and iron and perhaps calcium) . When cool, 10 cc. of saturated solution of sodium-ammonium-hydrogen phosphate shall be added with constant stirring. When the 1 Since this procedure does not involve the determination of silica, a second evaporation is'unnecessary. 8 SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. crystallin ammonium-magnesium orthophosphate has formed, ammonia shall be added in moderate excess. The solution shall be set aside for several hours in a cool place, filtered and washed with water containing 2.5 per cent of NH 3 . The precipitate shall be dissolved in a small quantity of hot hydrochloric acid, the solution diluted to about 100 cc., 1 cc. of a saturated solu- tion of sodium-ammonium-hydrogen phosphate added, and ammonia drop by drop, with constant stirring, until the pre- cipitate is again formed as described and the ammonia is in moderate excess. The precipitate shall then be allowed to stand about two hours, filtered and washed as before. The paper and contents shall be placed in a weighed platinum crucible, the paper slowly charred, and the resulting carbon carefully burned off. The precipitate shall then be ignited to constant weight over a Meker burner, or a blast not strong enough to soften or melt the pyrophosphate. The weight of magnesium pyrophosphate obtained multiplied by 72.5 gives the percentage of magnesia. The precipitate so obtained always contains some calcium and usually small quantities of iron, aluminum, and manganese as phosphates. Permissible 27. A permissible variation of 0.4 will be allowed, and all results in excess of the specified limit but within this permissible variation shall be reported as 5.00 per cent. Variation. VIII. DETERMINATION OF SPECIFIC GRAVITY. Apparatus. 28. The determination of specific gravity shall be made with a standardized Le Chatelier apparatus which conforms to the requirements illustrated in Fig. 1. This apparatus is stand- ardized by the United States Bureau of Standards. Kerosene free from water, or benzine not lighter than 62 Baume, shall be used in making this determination. Method. 29. The flask shall be filled with either of these liquids- to a point on the stem between zero and one cubic centimeter, and 64 g. of cement, of the same temperature as the liquid, shall be slowly introduced, taking care that the cement does not adhere to the inside of the flask above the liquid and to free the cement from air by rolling the flask in an inclined position. After all the cement is introduced, the level of the liquid will rise to some division of the graduated neck; the SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 9 (- 5cm ljNo|.A|J Ground Glass Stopper-'' c!c v \ 6cc Have two O.I cc Graduations extend above J and below Mark ----.> 17 cc 8 cm -H i [<- - 9cm >) FIG. 1. Le Chatelier Apparatus, . S 10 SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. difference between readings is the volume displaced by 64 g. of the cement. The specific gravity shall then be obtained from the formula Weight of cement (g.) Specific gravity = Displaced volume (cc.) 30. The flask, during the operation, shall be kept immersed in water, in order to avoid variations in the temperature of the liquid in the flask, which shall not exceed 0.5 C. The results of repeated tests should agree within 0.01. 31. The determination of specific gravity shall be made on the cement as received; if it falls below 3.10, a second deter- mination shall be made after igniting the sample as described in Section 20. IX. DETERMINATION OF FINENESS. Apparatus. 32. Wire cloth for standard sieves for cement shall be woven (not twilled) from brass, bronze, or other suitable wire, and mounted without distortion on frames not less than lj in. below the top of the frame. The sieve frames shall be circular, approximately 8 in. in diameter, and may be provided with a pan and cover. 33. A standard No. 200 sieve is one having nominally an 0.0029-in. opening and 200 wires per inch standardized by the U. S. Bureau of Standards, and conforming to the following requirements: The No. 200 sieve should have 200 wires per inch, and the number of wires in any whole inch shall not be outside the limits of 192 to 208. No opening between adjacent parallel wires shall be more than 0.0050 in. in width. The diameter of the wire should be 0.0021 in. and the average diameter shall not be outside the limits 0.0019 to 0.0023 in. The value of the sieve as determined by sieving tests made in conformity with the standard specification for these tests on a standardized cement which gives a residue of 25 to 20 per cent on the No. 200 sieve, or on other similarly graded material, shall not show a variation of more than 1.5 per cent above or below the standards maintained at the Bureau of Standards. Method. 34. The test shall be made with 50 g. of cement. The sieve shall be thoroughly clean and dry. The cement shall be SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 11 placed on the No. 200 sieve, with pan and cover attached, if desired, and shall be held in one hand in a slightly inclined posi- tion so that the sample will be well distributed over the sieve, at the same time gently striking the side about 150 times per minute against the palm of the other hand on the up stroke. The sieve shall be turned every 20 strokes about one-sixth of a revolution in the same direction. The operation shall continue until not more than 0.05 g. passes through in one minute of continuous sieving. The fineness shall be determined from the weight of the residue on the sieve expressed as a percentage of the weight of the original sample. 35. Mechanical sieving devices may be used, but the cement shall not be rejected if it meets the fineness requirement when tested by the hand method described in Section 34. 36. A permissible variation of 1 will be allowed, and all Permissible results in excess of the specified limit but within this permissible Vanatlon - variation shall be reported as 22 per cent. X. MIXING CEMENT PASTES AND MORTARS. 37. The quantity of dry material to be mixed at one time Method, shall not exceed 1000 g. nor be less than 500 g. The propor- tions of cement or cement and sand shall be stated by weight in grams of the dry materials; the quantity of water shall be expressed in cubic centimeters (l cc. of water = 1 g.). The dry materials shall be weighed, placed upon a non-absorbent surface, thoroughly mixed dry if sand is used, and a crater formed in the center, into which the proper percentage of clean water shall be poured; the material on the outer edge shall be turned into the crater by the aid of a trowel. After an interval of J minute for the absorption of the water the operation shall be completed by continuous, vigorous mixing, squeezing and kneading with the hands for at least one minute. 1 During the operation of mixing, the hands should be protected by rubber gloves. 38. The temperature of the room and the mixing water \ shall be maintained as nearly as practicable at 21 C. (70 F.). 1 In order to secure uniformity in the results of tests for the time of setting and tensile strength the manner of mixing above described should be carefully followed. At least one minute is necessary to obtain the desired plasticity which is not appreciably affected by con- tinuing the mixing for several minutes. The exact time necessary is dependent upon the personal equation of the operator. The error in mixing should be on the side of over mixing. 12 SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. XL NORMAL CONSISTENCY. Apparatus. 39. The Vicat apparatus consists of a frame A (Fig. 2) bearing a movable rod B, weighing 300 g., one end C being 1 cm. in diameter for a distance of 6 cm., the other having a removable needle Z), 1 mm. in diameter, 6 cm. long. The rod FIG. 2. Vicat Apparatus. Is reversible, and can be held in any desired position by a screw E, and has midway between the ends a mark F which moves under a scale (graduated to millimeters) attached to the frame A . The paste is held in a conical, hard-rubber ring G, 7 cm; in diam- eter at the base, 4 cm. high, resting on a glass plate H about 10 cm. square. SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 13 40. In making the determination, 500 g. of cement, with a Method, measured quantity of water, shall be kneaded into a paste, as described in Section 37, and quickly formed into a ball with the hands, completing the operation by tossing it six times from one hand to the other, maintained about 6 in. apart; the ball resting in the palm of one hand shall be pressed into the larger end of the rubber ring held in the other hand, completely filling the ring with paste; the excess at the larger end shall then be removed by a single movement of the palm of the hand; the ring shall then be placed on its larger end on a glass plate and the excess paste at the smaller end sliced off at the top of the ring by a single oblique stroke of a trowel held at a slight angle TABLE I. PERCENTAGE OF WATER FOR STANDARD MORTARS. Percentage of Water for Neat Cement Paste of Normal Consistency Percentage of Water for One Cement, Three Standard Ottawa Sand. Percentage of Water for Neat Cement Paste of Normal Consistency. Percentage of Water for One Cement, Three Standard Ottawa Sand. 15 9.0 23 10.3 16 9.2 24 10.5 17 18 19 9.3 9.5 9.7 25 26 27 10.7 10.8 11.0 20 9.8 28 11.2 21 22 10.0 10.2 29 30 11.3 11.5 with the top of the ring. During these operations care shall be taken not to compress the paste. The paste confined in the ring, resting on the plate, shall be placed under the rod, the larger end of which shall be brought in contact with the surface of the paste; the scale shall be then read, and the rod quickly released. The paste shall be of normal consistency when the rod settles to a point 10 mm. below the original surface in \ minute after being released. The apparatus shall be free from all vibrations during the test. Trial pastes shall be made with varying percentages of water until the normal consistency is obtained. The amount of water required shall be expressed in percentage by weight of the dry cement. 41. The consistency of standard mortar shall depend on the 14 SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. amount of water required to produce a paste of normal con- sistency from the same sample of cement. Having determined the normal consistency of the sample, the consistency of stand- ard mortar made from the same sample shall be as indicated in Table I, the values being in percentage of the combined dry weights of the cement and standard sand. XII. DETERMINATION OF SOUNDNESS. 1 Apparatus. 42. A steam apparatus, which can be maintained at a tem- perature between 98 and 100 C., or one similar to that shown in Fig. 3, is recommended. The capacity of this apparatus may be increased by using a rack for holding the pats in a vertical or inclined position. Method. 43. A pat from cement paste of normal consistency about 3 in. in diameter, J in. thick at the center, and tapering to a thin edge, shall be made on clean glass plates about 4 in. square, and stored in moist air for 24 hours. In molding the pat, the cement paste shall first be flattened on the glass and the pat then formed by drawing the trowel from the outer edge toward the center. 44. The pat shall then be placed in an atmosphere of steam at a temperature between 98 and 100 C. upon a suitable sup- port 1 in. above boiling water for 5 hours. 45. Should the pat leave the plate, distortion may be detected best with a straight edge applied to the surface which was in contact with the plate. XIII. DETERMINATION OF TIME OF SETTING. 46. The following are alternate methods, either of which may be used as ordered: Vicat 47. The time of setting shall be determined with the Vicat Apparatus. apparatus described in Section 39. (See Fig. 2.) Vicat 48. A paste of normal consistency shall be molded in the Method, hard-rubber ring G as described in Section 40, and placed under 1 Unsoundness is usually manifested by change in volume which causes distortion, cracking, checking or disintegration. Pats improperly made or exposed to drying may develop what are known as shrinkage cracks within the first 24 hours and are not an indication of unsoundness. These conditions are illustrated in Fig. 4. The failure of the pats to remain on the glass or the cracking of the glass to which the pats are attached does not necessarily indicate unsoundness. SPECIFICATIONS AND TESTS FOR PORTLAND CEMENT. 15 ijT )?I II! ,