-Y‘-’ i n _— —— —— —— —— —— —— —_——- —- _———- —— —— —— —— —— — THESIS A COMPARITWE ANALYSIS or MICHIGAN CEMENTS 7 ' Donald C. Godfrey & M. Frank Bornor ~ ‘ I924 1 1 1 1.51. in! I. , 1 -llibll.l--.-. 1 1. . ..: H..-,. .. . . .. _ . u . . . . . \ . ‘1 .. . . l . . . . , 1 .. ....,3.. T ,......v. . .2. 1,1. ‘. . . . . . ...... 1 . - .. A..- . ....1 \II .11.. 11.1.1-1... ....,..... .t..- 3.711 .. ....| .., u ,. 111. .u,..J .. ha}...i.. . T: r . .. .. A. w.;..g.............n Art 1. . . .. .. .1.) a . i... 1p: . .. , v.2, ... $12.11.}. 1.. 72.5 . .1 1. :u . .3“. «H517 u. . ..... r .r » {HLLuKnUmrflnrJlrh..H.\m:....1r.. . .3 .1 .s..“1,.,1r.....vr.2.r...._... Kauai".wharmw§kfl.5wuuLu.‘.l._Irruryvv?r.l{v 31,. Ivr.~FrrrJ1. . . ‘ I‘ 5“. . _ 1 , . 1 u x , V . .. . i 4, .. . ‘9 1 .. c y. x T [A . It! .. . .2 THESIS to {a \ “IV . , J 1.. i I... _ 2:... . L»: .;. . _. . .- V . Ia. . . nfmimma...:«3.? . . . w . . . .. ... ....... .. . .. . .. . ; , r. .. skits ...... . ..... 1| w)..\......vs..rl.r.ia:.. .. 1.1.2.1? $21. . . .1...l\..: . . 3.1:»..37. . 2....Itt....i.lfu§u.¥h. ..1.......:.. . A CUJPARIQIVJ ANALYSIS OF MICEchH chgmrs A Thesis Submitted to the Faculty of Michigan Agricultural College by '\ ‘_—- \1 fl -\ ‘ fl (1' -,~‘ \ Donald C! Godfrey and M. Frank Bornor Candidates for Degree of Bachelor of Science June, 1964. JHESIF The authors of this book are very thankful to Professor Voddor, instructor, counsellor, and friend for his advice and help in the preparation of this volume. We are also very grateful to Professor Allen for his helpful Suggestions, advice, and information concerning tests. Professor Allen has vary kindly agreed to chrry on tests for tensile strength for the poriods which we are unable to complote. The Authors. HIsTUhY. A curious, groat bridge which has come down from tho days of the ancients stands in the south If Franco, not far from the old city of Nimos. It is called the Pont du Gard and it is still referred to by the natives of tho region as one of tho sovon wonders of thw world. It spans tho doop valley of the Gard and it is builded in three tiers of stone arches. There are six arches of tho lowost tier. ranging frma sixty to soventy~fivo feet in width, eleven seventy- fivo foot arches in tho cocond tier, and thirty-five smaller ones in the third, carrying tho sc-callod "spoons", or water trough, through which tho Romans twenty centuries ago were wont to supply tho fountains of their beloved Henaunua, about a dozen miles distant. It is this trough that tho Emperor Augustus once lined with cement. Today, after twenty conturios, that lining remains one of tho hardest substances in the world. The many yoars that it actually carried water only added to tho encasing. The secretions of line from tho water itself gradually narrowed tho spoons until today, many centuries after tho Pont do Gard was abandoned as an aqueduct, one finds that in places it is hard to valk through the narrowed space. In the latter days of the umpire, the Romans grew extremely expert in the use of a form of concrete. They awoke gradually to the tenacious powers of lime rock, and before the great fabric of their high civilization crumbled, they were working quite extensively in a fabric that would outlivo many civilizations-in a plastic stone that would not and could not crumble. The traces of their work in natural cement are still existent everywhere within the lands that they once occupied. Their day was the early dawn of the Concroto Ago, For nineteen centuries the Concrete Age, although born, lingered in a dreary immaturity. For it was not until about one hundrod years ago that an Englishman - Joseph depdin of Leeds - invented Portland Cement, so naming it from a widely used building stone from the Isle of Portland, to which his invention, once thoroughly set, bore a close resemblance in color. Aspdin's method was through application to the cement raw materials of an intense heat. It had been of course, the traditional custom to burn the lime rock, to complete through fire the transformance of its carbonate of lime to an oxide of lime. But the kilns were crude and the process simple. moreover, no matter how carefully one ground the rock before pouring it into the kilns, there was bound to result great quantities of hard slag, or "clinker", as it became known to the lime burners. This was sifted out from the finished product and thrown away. hut its very presence was a constant annoyance. Into nepdin's mind there flashed the thought one day, a century ago, that perhaps the despised clinker might possibly contain certain cement qualitios of real value. He began unperimenting with it, pulverizing it into the finest sort of powder, and mixing it with water and a variety of aggregates of sand and stone. It responded to the tests. It made an artificial rock, of an appearance and a quality far superior from that obtained through the natural cement, with the clinker carefully eliminated. Aspdin went further. Ho experimented with heats much in excess of those previously in use in limo-kiln practice upon lime rook, until the product of the kiln was entirely clinker, which was just the thing he really desired. Aspdin's chief contribution was not in tle advanced use which he made of the clinker, but rather that he was the first one to realize the importance of the preper mixture of the materials ~-he made a science of the entire business. But elen.with his work done, portland cement did not come into its own quickly. For while it was used in many parts of england and France as long ago as the 'fifties', it was not until 1870 that long eXpernnents were made to produce portland cement in the United States. Yet, once invented, pcrtland cement moved but slowly toward the fulness of its possibilities. The process for its production was so intricate, the mechanisms for carrying out the process so much more complicated than those recuired for the production of natural cement or for slacking lime that men passed it by. Then, about a quarter of a century ago, some things began to happen. First and foremost important of all, prices of material things in the United States began to go up, as well as labor. This was especially true in the case of building materials, all Save cement, in which there was a decided lowering of price, due in a large measure to the introduction of the rotary kiln. To an appreciable extent the Concrete Age has come into its own through dire labor necessities. The fact that in this day and age we of the United States are long in electricirns and patsge helpers and very short in good masons - either brick or stone - has been a powerful factor in its recent great growth. In 1896 the annual production of portland cement in this country first reached the then tremendous figure of a million barrels. Yet this was but a beginning. Four years later - at the beginning of the present century - it had come to 8,482,000 barrels in a single twelvemonth. These were still mere beginnings. In 1920 more than 100,000,000 barrels of portland cement were manufactured in the united States. In 1922 the production was nearly 116,000,000 barrels. The Concrete Age has truly arrived. The above is an extract from "Observations on an Outstanding American Industry" by Edward Hungerford. The History of the Cement Industry in Michigan. fihe first attenpt to manufacture portland cement in the united States was made in Michigan in.1872, when an experio mental vertical kiln plant was constructed in Kalamazoo, using marl and clay in the process. The venture was a failure and exercised little or no influence in the New York and Pennclyvania developments beginning in 1875. After the failure of the Kalamazoo venture, no second attempt was made to re-establish the industry in Michigan until 1896 in which year the Peerless Portland Cement Cc. erected a vertical kiln plant at Union City, Branch county, and began the successful manufacture of portland cement from.narl and shale. In 1897 the Bronson Portland ceaent co. erected a plant aat Bronson, Branch county, and in 1898 the Goldwater Decent Company, now the Wolverine Portland Cenent 00., built plants at Goldwater and Quincy. third In 1900 Michigan with six plants attained fix n place in the production of cement in the United states. since 1896, thirty-six different cement plants have been projected or built in Michigan and eleven are in operation today. 0f the elwven plants, five are reported to be using marl and clay, five using lime stone and clay or shale, and one using clay and the waste from the plant of the Hichigan Alkali Co. All plants use scal as fuel, nine manufacture cement by the "wet process” and two by the dry process. The Petoskey plant which was erected on the limestone deposits on Little Traverse Bay is pronounced ”the best and most efficient wet process plant".-Geologioa1 Report for Jichigan prior to 1921. The boom years of the cement industry in uiohigan were between 1899 and 1901, the production growing from less than $50,000 barrels in 1899 to more than 1,000,000 barrels in 1901. By 1920 the production had increased to more than 4,000,000 barrels per year. In 1920 Michigan stood seventh in the production and shipment of cement. OBJECT. This thesis was taken up by the authors with two objects in View: First, to determine if all the brands of Portland Cement manufactured in Michigan are made to conform.to the standard specifications of the American Society fer Testing Materials. Second, to determine if possible from results obtained if there is any marked preference between the different brands of cement as to their quility and fitness, and if so in our opinion, which brand this is. In order to insure that a fair sample of each brand would be secured, three sacks of each were obtained, Atlas and Universal brands of cement were used as a controls because of their long standing as being among the best portland cements manufactured in this country. DEFIHITION. 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 cal- cination excepting water and calcined or uncalcined gypsum. SPECIFICATIONS. The specifications used are those oifthe American Society for Testing Materials and are of two distinct parts, Chemical and Physical. Chemical Properties. Loss on ignition. Per cent eeeeeeeeeeeeeeeeeeeeeeee 4000 InBOInblo residue, per Cent........................ 0.85 Sulphuric unh dridc (303) per cent................. 2e00 Mfl8n881l (M80 9 Per con¥ceeeeeceececeeeeeeOeceeeece 5000 These limits are not to be exceeded. Physical Properties. 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 say be made upon an ignited sample. The specific gravity test will not be made unless specifically ordered. The residue on a standard No. 200 sieve shall not exceed 22 per cent by weight. A pat of neat cement shall remain firm and hard, and show no signs of distortion, cracking, checking, or disintegra- tion in the steam test fer soundness. The cement shall not deveIOp initial set in less than 46 minutes when the Vical needle is used or 60 minutes when the Gillmoro needle is used. Final set shall be attained within 10 hours. The average tensile strength in pounds per square inch of not less than three standard mmrtar briquettes composed of one part cement and three parts standard send, by weight, shall be equal to or higher than the follmring: Age at Test Tensile Strength Days Storase of'Briquettes lb. per 81. in. 7 1 day in moist air, 6 days in water 200 28 1 day in moist air, 27 days in water 500 The average tensile strength of standard mortar at 28 days shall be higher than the strength at 7 days. SAIPLING. Tests may be made on individual or composite sanples as may be ordered. Each test sample should weigh at least 8 pounds. I The samples ior tests made in this thesis were made by taking a 3000p full from each sack and thoroughly mixing. The sample used in the test was then taken from this mixture. The average weight of cement taken from each sack was about 6 pounds making the total sample about 15 pounds. CHEJICAL ANALYSIS. Loss on Ignition. Method. One gram of cenent shall be heated in a weighed covered platinum crucible, of 20 to 25 cc. capacity, as follows: The crucible shall be placed in a hole in an asbestos hoard, 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 irom the hole in the board. Greater neatnees and shortening of the time of heating are secured by making a hole to fit the crucible in a circular disk of sheet platinum and placing the disk over a somewhat larger hole in an asbestos board. A permissable variation of 0.25 will be allowed, and all results in excess of the specified limit but within this pernissable variation shall be reported as 4 per cent. Remarks: In making this test in this thesis we were unable to get the platinum crucibles and fused silica crucibles of the specified size were used in their place. In heating the cement we made one blast of one-half hour rather than the two heats of 15 minutes and 5 minutes as specified. From our conversations with Chief Chemists at some of the plants in lichigan we found that this is the method that is used altogether in commercial testing. Insoluble Residue. met-1106. e To a 1 gram sample of cement shall be added 10 cc. of water and 5 cc. of concentrated hydrochloric acid; the liquid shall be warned 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 percent solution of sodium carbonate, the liquid being held at a temperature Just short of boiling for 15 minutes. The remaining residue shall be filtered, washed with cold water, then.with a few drops of hot hydro- chloric acid, 1:9, and finally with hot water, and then ignited at a red heat and weighed as the insoluble residue. A permisaable variation of 0.15 will be allowed, and all results in excess of the specified limit but within this permissable variation shall be reported as 0.85 per cent. Remarks: This test is very seldom made except on the re~chcck of cement which has been.reJected. Statement made by Chief Chemist of a large cement company which has plants in several states, to the authors of this thesis. Sulphuric Anhydride. Method. One gram of the cement shall be dissolved in 5 cc. of concentrated hydrochloric acid diluted wit; 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 pre- cipitate is well formed. The solution shall be digested on the steam.bath until the precipitate has settled. The precip~ itate shall be filtered, washed, and the paper and contents placed in a weighed platinum crucible and the paper slowly charred and consumed without flaming. The barium sulphate shall then be ignited and weighed. The weight obtained multiplied by 34.3 gives the percentage of sulphuric 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. A permissable variation of 0.10 will be allowed, and all results in excess ef the specified limit but within.this permissable variation shall be reported as 2.00 per cent. Remarks: In making this test the authors used 10 cc. of concentrated hydrochloric acid and 10 cc. of water te dissolve the cement in instead of 6 cc. of each as specified. The authors spent one day in working and studying methods used in chemical analysis in a cement plant and we found that they used the amounts stated. The extra amounts used would of course have no effect on the amounts of constituents found, being used only to dissolve the cement. Magnesia. Method: To 0.6 gram of the cement in an evaporating dish shall be added 10 cc. of water tp prevent lumping and then 10 cc. of concentrated hydrochloric acid. The liquid shall then then be gently heated and agitated until attack is complete. The solution shall be evaporated to complete dryness on a steam ornater bath. Tc hasten dehydration the residue may be heated to 106 or even 200° 0. for one half to one hour. The residue shall be treated with lOcc. of concentrated hydrochloric acid diluted with an equal amount of water. The dish shall be covered and the solution digested for ten minutes on a steam bath or water bath. The diluted solution slall be filtered and the sep- arated silica washed thoroughly with water. rive 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 250cc). This shall be made alkaline with ammonium hydroxide, boiled until there is but a faint odor of ammonia, and the pre- cipitated iron and aluminum hydroxides. after settling, shall be washed with hot water, once by decantaticn and slightly on the filter. Setting 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 hydroxides of iron and aluminum, reduced in volume if need be, 1 cc. of almonium 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 line shall then be repricipitated by ammonium oxalate, allowed to stand until settled, filtered and washed. The combined filtrates from the calcium precipitates shall be acidified with hydrochloric acid, concentrated on the steam bath to about 150 co., 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 solu- tion of sodium-ammonium-hydrogen phosphate shall be added with constant stirring. When the crystallin ammonium- magnesium orthOphosphate has formed, ammonia shall be added in moderate excess. The solution hhall be set aside for several hours in a coil plate, filtered and washed with water containing 2.5 per cent of Bug. The precipitate shall be dissolved in a small quantity of hot hydrochloric acid, the solution diluted to about 100 co., 1 cc. if a saturated solution of sodium-ammonium- hydrogen phosphate added, and ammonia drop by drop, with constant stirring, until the precipitate 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 precipi- tate shall then be ignited to constant weight over a Hekerr burner, or a blast not strong enough to soften or melt the perphosphate. The weight cf’magnesium pyro- phosphate cabtined multiplied by 72.5 gives the percentage of magnesia. The precipitate so obtained always contains some calcium and usually small quantities of iron, alum- inum, and manganese as phosphates.~ A permissable variation of 0.4 will be allowed, and all results in excess of the specified limit but within this permissable variation shall be reported as 5.00 per cent. Remarks: In our tests for'magnesia we did not perform the second precipitation and filtration as is called for in some places in this test. We followed more closely the method used in commercial practice which is the same in all ways except the second precipitation. In "Portland Cement" by Head, in chapter on "Tests" the method is also given which does not call for the second precipi- tation but which is the same in all other respects. The time required for a magnesia test previous to the cooling of the solution is somewhat over four hours, therefore ‘we believe our course in ommtting the parts mentioned is Justifigd” inasmuch as we only had four hours in a continuous period in which to perform this test. TABLL'J OF RESULTS OF CHMICAL TESTS. dices on *Thscluhle Brand Ignition Residue Sulphuric magnesia Anhydride (ago) Atlas 2.41 .66 1.72 3.67 Alpha .90 .70 1.18 1.66 Huron 1.41 .84 1.85 3.28 New Astna 1.00 .85 2.00 2.34 Newaygc .85 .64 1.80 3.84 New Egyptian 1.40 .85 1.08 3.26 Peerless .73 .72 1.71 3.44 Petoskey 1.48 .76 1.92 03.91 Peninsular .86 .85 1.74 3.93 Michigan 2.10 .76 1.95 3.76 hyandotte 1.25 .85 1.86 2.72 Wolverine 1.16 .74 1.36 3.97 Universal 1.71 .73 1.40 4.02 As the above table shows, all of the Michigan cements come well under the specifications required by the American Society for Testing Materials, as to chemical analysis. The results given should not be considered as being absolute, but they may be considered as being comparitive as all tests were run under the same conditions and with the same degree of accurateness throughout the entire tests. In the tests all computations were carried to the fourth place except in final result which was reduced to two decimal places as shown. PHYSICAL ANALYSIS Determination of Specific Gravity. Apparatus: The determination of specific gravity shall be made with a standardised Le Chatelier apparatus. This apparatus is standardized by the united States Bureau of Standards. [Kerosene free from water, or beneine not lighter than 62° Baume'. shall be used in making this determination. .Method: The flask Ihall be filled with either of these liquids to a point on the stem between zero and one cubic centimeter, and 6e 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 difference between readings is the volume displaced by 64 g. of the cement. The specific gravity shall then be obtained from the formula ‘ :: Heisbi-ef-csccnt. .a 1-.. Sp.°111° gravity Diaplaced volwme cot) The flask, during the Operation, shall be kept immersed in water, in order to avoid variations in the temp- erature of the liquid in the flask, which shall not exceed 0.50 0. The result of repeated tests should agree within 0.01 The determination of specific gravity shall be made on the cement as received; if it falls below 3.10, a second determination shall be made after igniting the sample as in the test for Loss on Ignition. Remarks: In making this test the authors used kerosene free from water for the liquid. The kerosene was placed in the flasks and allowed to stand in water for one day before it was used. The few samples of cement which did not at first pass this test went well under the test after the sample had been ignited. Determination of Fineness. 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 1% 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. A standard No. 200 sieve is one having nominally an 0.0029 in. Opening and 200 wires per inch standardized by the U. 8. Bureau of Standards, and conforming to the follow- ing requirements: The No. 200 eieee 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. Ho 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 seiving tests made in conformity with the standard specifications for these tests on a standardized cement which gives a residue of 25 to 20 per cent on the ha. 200 seive, 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. .Hethod: The test shall be made with 50 g. of cement. The seive shall be thoroughly clean and dry. The cement shall be placed on the No. 200 seive, with pan and cover attached, if desired, and shall be held in a slightly inclined posi- tion so that the sample will be well distributed over the seive, 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 seive shall be turned every 25 strokes about one-sixth of a revolution in the same direction. The Opera- tion shall continue until not more than 0.05 3. passes thru in one minute of continuous seiving. The fineness shall be determined from the weight of the residue on the seive expressed as a percentage of the weight of the original sample. Mechanical seiving devices may be used, but the cement shall not be rejected if it meets the fineness requirements when tested by the hand method Just described. hemarks: In making this test the authors used the hand method described in all cases. Mixing Cement Pastes and Hortars. The quantity of dry material to be mixed at one time shall not exceed 1000 3. nor be less than 600 g. The preportions 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. 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 s trowel. After an interval of 5 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. During the Operation of mixing, the hands should be covered by rubber gloves. The temperature of the room and the mixing water shall be maintained as nearly as practicable at 21° 0 (70° F). Remarks: In mixing the mortar used in these tests the temperature of the water was kept as nearly as possible at 21° 0. but the temperature of the room could not be controlled and there was much variation. Normal Consistency. Apparatus: The Vicat apparatus consists of a frame bearing a movable rod, weighing 300 g., one end being 1 cm. in diameter for a distance of 6 om., the other having a removable needle, 1 mm. in diameter, 6 cm. long. The rod is reversible, and can be held in any desired position by a screw, and has midway between the ends a mark ahich.moves under a scale attached to the frame. The paste is held in a conical, hard-rubber ring, 7 cm. in diameter at the base, 4 cm. high, resting on a glass plate about 10 cm. square. In making the determination, 500 g. of cement, with a measured quantity of water, shall be kneaded into a paste, as described previous to this, 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 and 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 and on a glass plate and the excess paste at the smaller and sliced off at the tsp of the ring by a single oblique stroke of a trowel held at a slight angle 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 larger and of the rod, the end of the rod brought in contact with the paste; the scale shall then be read and the rod quickly released. The posts shall be of normal consistency when the sod settles to a point 10 mm. below the original surface in % minute after being released. The apparatus shall be free from 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. The consistency of standard mortar shall depend on the amount of water required to produce a paste of normal consistency from the same sample of cement. Having deter- mined the normal consistency of the sample, the consistency of standard mortar‘made from the same sample shall be as indicated in the following table, the values being in per- centage of the combined dry weights of the cement and standard sand. PERCENTAGE OF MATER FOR STANDARD HORTARS. §ercentage of’hater Percentage ofrhater for Heat Cement for One Cement, Paste of Normal Three Standard Ottaaa Consistency ,, Sand. hp ' 15 9.0 :: 23 10.3 16 9.2 SE 24 10.5 17 ' 9.5 E; 25 10.7 13 9.5 22 25 10.8 19 _ 9.? £2 27 11.0 20 9.8 E; 28 11.2 21 10.0 E? 29 11.3 22 10.2 E2 30 11.5 The Vicat apparatus seems to be used very little in cement plant labratories. The men who do the testing every day prefer the ball method for testing for normal consist- ency . It is clained by them that their results are more accurate than with the Vicat apparatus. It is interesting to note that our results for normal consistency were higher in nearly every case than the normal consistency used for testing at the plants with which we came in contact. 16 Determination of Soundness. A steam apparatus, which can be maintained at a temperature between 98 and 1000 C. is recommended. The capacity of this apparatus may be increased by using a rack for holding the pets in a vertical or inclined position. A pat of cement paste of normal consistency about 3 in. in diameter, % 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. he 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. The pat shall then be placed in an atmosphere of steam at a temperrture between 98 and 100° 6. upon a suit- able support 1 in. above boiling water for 5 hours. hhould 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. Determination of Time of Setting. The Gillmore needles were used in making this test. .Method: The time of setting shall be determined as follows: A pet of neat cement paste about 3 in. in diameter and % in. in thickness with a flat tap, mixed to a normal consistency, shall be kept in moist air at a temperature maintained as nearly as practicable at 21° C. The cenent shall be considered to have acquired its iritial set when the pet will bear, without appreciable indentation, the Gillmore needle 1/12 in. in diameter, loaded to weigh a; pound. The final set has been acquired when the pat will bear without app- reciable indentation, the Gillmore needle 1/24 in. in diameter, loaded to weigh 1 pound. In making the test, the needles shall be held in a vertical position and applied lightly to the surface of the pat. The initial set should not be acquired in less than 60 minutes with the Gillmore needle, and the final set should be acquired within 10 hours. Tension Tests. In making briquettes for tension tests the gang molds were used. Molds were cleaned before use and oiled enough to prevent cement from sticking to the sides. The molds shall be made of nonpcorroding metal and have sufficient material in the sides to prevent spreading during molding. The sand to be used shall be natural sand from Ottewe 111,, screened to pass a No. 20 sieve and retained on a No. 30 sieve. This sand, having passed the No. 20 sieve. shall be considered standard when not more than 6 3. pass the No. 30 sieve after one minute or continuous sieving of s 500 3. sample. The 81.703 shall conform to the following specifica- tions: The No. 20 sieve shall have between 19.5 and 20.5 wires per whole inch of the warp wires and between 19 and 21 18 wires per shole inch of the shoot wires. The diameter or the wire should be 0.0165 in. and the average diameter shall not be outside the limits of 0.0160 and 0.0170 in. The No. 50 sieve shall have between 29.5 and 30.5 wires per whole inch of the warp wires and between 28.5 and 31.5 wires per whole inch of the shoot wires. The diameter of the wire should be 0.0110 in. and the average diameter shall not be outside the limits 0.0105 to 0.0115 in. Immediately after mixing, the standard mortar shall be placed in the molds, pressed in firmly with the thumbs and smoothed off with e trowel without reaming. Additional mortar shall be heaped above the mold and smoothed of! with e trowel; the trowel shall be drawn over the mold in such a manner as to exert a moderate pressure on the materiel. The mold shall then be turned over and the Operation of beeping, thumbing and smoothing of! repeated. Tests shall be made with any standard machine. The briquettes shall be tested as soon as they are removed from the water. The bearing surfaces of the clips and briquettes shall be free from grains of sand or dirt. The briquettes shall be carefully centered and the lead applied continuously at the rate of 600 lb. per minute. Testing machines should be frequently calibrated in order to determine their accuracy. Briquettes that are manifestly faulty, or which give strengths differing more than 15 per cent from the average value of all test pieces made from the same sample and ‘broken at the same period,-shall not be considered in deter- ruining the tensile strength. Remarks: As the tensile strength is watched very closely by persons buying cement and as this is one of the most important tests we were very careful to see that all clips and briquettes were perfectly clean and that rells were oiled. In no cases did the briquettes break in such a way as to appear due to dirt or grit on the machine or hrieuette. Storage of Test Pieces. The moist closet may consist of a soapstone, slate or concrete box, or a wooden box lined with metal. I! a wooden box is used, the interior should be covered with felt or broad wicking kept wet. The bottom of the moist closet should be provided with non-absorbent shelves on which to place the test pisses, the shelves being so arranged that they may be withdrawn readily. Unless otherwise specified all test pieces, immediately after molding, shall be placed in the meist closet, for from 20 to 24 hours. The briquettes shall he kept in molds on glass plates in the moist closet for at least 20 hours. After 24 hours in moist air the briquettes shall be iumersed in clean water in storage tanks of non-corroding material. The air and water shall be maintained as nearly as practicable at a temperature of 210 C. ( 70°F). Remarks: All test pieces were stored as specified except that we could not keep the air and water at the desired temperature. lhis may have had some effect on the tensile strength, but all briquettes were in the same storage tank so that the results are strictly comparative. Brand Alpha Atlas huren Michigan New Aetna Newaygo RASJh Specific Gravity 5.14 Jelfi 3.09 *3.23 3.06 3.20 3.08 *3.16 3.10 New Egyptian 3.10 Peerless Peninsular Petoskey Universal Wolverine Wyandotte 5.11 3.07 *3.18 3.08 *3.21 3.06 *3.17 3.16 3.13 l % 8518 80.7 81.6 80.6 81.4 80.4 85.7 78.04 85.6 89 3 CF PAYEICAL Tails. Eineness Soundness OK Normal Consist. 26.75 24.5 28.5 27 26 23.5 24.5 * Refers to the test made for specific gravity after the sample had been ignited for 45 minutes. 21 Brand Alpha Atlas Huron Michigan New Aetna Rewaygo Haw Egyptian Peerless Peninsular Petoskey universal Wolverine Wyandotte RfidJLTS TIJ£ OF $3? Initial ‘ 4 2 4 4 5 5 4 3 4 I 5 02' hrs. hrs. hrs. hrs. hrs. hrs . hrs. hrs. hrs. hrs. hrs. hrs. hrs. 59 16 15 20 15 19 35 56 25 28 min. min. min. min. min. min. min. min. min. min. min. min. min. “OOQOQ'OQQQQU‘D Final Set hrs. 24 min. hr. 82 min. hrs. 6 min. hrs. 50 min. hrs. 8 min. hrs. 16 min. hrs. 8 min. hrs. 40 min. hrs. 82 min. hrs. 23 min. hrs. 45 min. hrs. 00 min. hrs. 23 min. From the above results it is seen that all brands come well within the limits of 60 minutes to 10 hrs. Brand Alpha AV. AVe Atlas 11? e Huron AV. Mich igan 41V 0 New Aetnu Av. Nevaygc AVe p 21?. Peerless T305101 STRSHGIH TJS S. 220 220 300 250 240 275 266 255 Cyptien.245 200 240 210 224 240 250 185 AVe 218 Period 28 day 3 mo. 6 mo. 9 m0. 1 yr. 560 500 515 525 0.55 275 310 505 506 505 555 825 000 005 525 326 TJNSILfi STRENGTHS. (Continued) Period Brand 7 day 28 day 5 mo. 6 mo. 9 mo. 1 yr. Peninsular 265 365 230 560 £55 320 295 360 Av. 266 551 Petoskoy 250 320 295 340 290 305 310 355 AVe 286 330 universal 260 280 210 315 180 315 -- 550 Av. 216 515 Wolverine 180 280 200 270 190 280 190 260 AVe 192 272 Wyandott e l90 .9 735’ 180 .2 7 o” 210 .244 vi; 230 .283 Av. 202 .c? 7‘? GJNERAL REflARKS. It was the original intention of the authors to make a complete analysis or the chemical prepertiee oi’ the cements which would include determination ci’ silica, iron and alminm, calcium, and magnesia. This would have nade a more complete comparison possible. Due to lack of time we were forced to abandon this idea after a few had been oompletly malyaed. Cements high in alminua reach their full strength in less time than low aluminum cements. With a complete analysis we might have been able to predict with some degree of accuracy how the curve of tensile strengths would appear for a period of one year. Without this analysis not much can be said with only the 7 and 28 day tests coupleted. G-ents high in aluminum also set quicker than low aluminum cements. Cnents which are high in silica are slow setting but show a good tensile strength, also a progressive gain in tensile strength. It was our intention, with a complete chemical analysis, to check the percentage of silica against the time of setting. CONCLUSION. In making our conclusions, since all brands passed the specifications required in all tests except tensile strength, and since this test together with soundness is watched most closely by purchasers of cement, we are using these tests as a basis for comparison. is all the cements passed the soundness test in a satisfactory manner, this makes the comparison rest on the tensile strength. The Newaygo brand of cement shows a high tensile strength for the seven and 28 day tests, in which the 28-day test shows a considerable increase over the 7-day test. The result of the time of setting shows very good for working conditions. The Alpha brand of cement shows a very high 7-day strength but there is no gain in the 28-day strength. The Wolverine brand of cement is the only one which failed in tensile strength. This brand failed in both the 7-day and 28-day tests. Seven of the eight briwuettes failed to come up to the required strength. 0 All of the.Michigan brands of cement, with the one exception, appear to stand up very favorable in comparison with the two eastern brands used in these tests, and passed all the specifications required by the American Societh for Testing Materials. 0". §~é;:£"‘i;3;".a USE GNU" :hll III .er'...:.|.|vfiq'w... .‘1Itllved ) fiflj.‘ L. .y‘lul 4 . e. . , . . u _ o , J h . . .. l . W 6 >A’E.-‘étvlvult$\tLll¢II.l.7 Liel(l1uyinl.f,‘1tolt ‘ ..‘\lJ«. l..l!.1|§o .allt 11".‘II‘ l1|)1.l‘t“tl,f1x\. 711.141)!l;a\ltllo“la1 I (‘Ill ‘1 "'TITI'ITIEJHILEMILITHljz't‘slitflffl'fljnflflalflflfiflmm“