THE REACTION OF CALCIUM CARBIDE 
 AND FERRIC OXIDE 
 
 ISADORE FINKELSTEIN 
 
 THESIS 
 
 FOR THE 
 
 DEGREE OF BACHELOR OF SCIENCE 
 
 CHEMISTRY 
 
 COLLEGE OF LIBERAL ARTS AND SCIENCES 
 
 UNIVERSITY OF ILLINOIS 
 
 1922 
 
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UNIVERSITY OF ILLINOIS 
 
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 May__ 3 _U 192^— 
 
 THIS IS TO CERTIFY THAT THE THESIS PREPARED UNDER MY SUPERVISION BY 
 
 Isadore Finkelateln 
 
 ENTITLED THE_REAGTipN_OF_ CALC_Il^ _Ci^ 
 
 IS APPROVED BY ME AS FULFILLING THIS PART OF THE REQUIREMENTS FOR THE 
 
 DEGREE OF 
 
 in CHEMISTRY 
 
 Instructor in Charge 
 
 Approved : 
 
 ACTING head of department of chemistry 
 
 
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ACKNOWLEDGMSNT 
 
 The writer wishes to express his appreciation and 
 sincere thanks to Dr. W. S. Putnam for his assistance in 
 the experimental work and writing of this thesis. 
 
Digitized by the Internet Archive 
 in 2015 
 
 https://archive.org/details/reactionofcalciuOOfink 
 
TABLE OP CONTENTS 
 
 Pages 
 
 Introduc tion 
 
 
 Historical 
 
 2-5 
 
 Experimental 
 
 6 -12 
 
 Conclusions 
 
 13 
 
 Note 
 
 14 
 
 Bibliography 
 
 15 
 
INTRODUCTION 
 
 This work was done in connection with that of W. J. 
 Farrel on the Desulphurization of steel by calcium carbide. 
 The purpose of the work to be described was to determine 
 whether or not calcium carbide will react as a reducing agent 
 in case oxides were present in the steel and to what degree 
 the reduction is carried out. S. Cohen has done work on the 
 reaction of calcium carbide and ferrous sulfide. The results 
 of the men mentioned above along with the results obtained in 
 this paper may be considered as one, and thus give a compre- 
 hensive report on the effects of calcium carbide as a desul- 
 phurizing and deoxidizing agent. The great need in the steel 
 industry, is a method to eliminate sulphur and phosphorus 
 from steel without the electric furnace temperatures. The 
 conditions of the investigation do not duplicate those of the 
 open hearth furnace, but it was undertaken with the hope of 
 learning something more than is Imown about the chemical 
 activity of CaC2 that could be applied in making steel. 
 

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2 
 
 HISTORICAL 
 
 Calcium Carbide was first detected by ^Bhler in 1862, 
 
 On heating a Ca-Zn alloy with carbon at a high temperature he 
 obtained a hard substance with a metallic luster, which be- 
 came grey on exposure to the atmosphere. The discovery of 
 Calcium Carbide is usually accredited to Moissoa, who prepared 
 it in an electric furnace. He heated coal and calcium oxide 
 at temperatures up to about 2000 degrees C and obtained the 
 carbide. The carbide is formed according to the equation 
 given below: 
 
 CaO 4 3C = CaC 2 4 CO 
 
 The present day manufacture of Calcium Carbide is 
 according to the equaltion given above. The carbon is in the 
 form of finely powdered coal. Care is taken that the coal 
 is of low sulphur content. This is necessary in order to 
 prevent formation of hydrogen sulfide when the carbide is used 
 for the preparation of acetylene gas. The first and largest 
 use for the carbide is in the production of acetylene. 
 
 CaCg 4 H 2 O = C 2 H 2 4 Ca(0H)2 
 
 Calcium carbide according to Erlwein, (1) Wrath and 
 Bentner will decompose very slowly. These men did extensive 
 work on the decomposition of the carbide by heat. Their re- 
 sults show that when CaC 2 is heated to 1000® C slow decompos- 
 ition takes place. They did not identify the product formed, 
 but assumed it to be a subcarbide of calcium. No metallic 
 

 
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3 
 
 calcium could be detected. On treatment with water no acety- 
 lene was evolved, but when nitrogen was passed over the 
 material the compound CaCN2 was formed. They showed that after 
 heating CaC2 for 10 hours at lOOO^C the carbide analyzed 
 36.6^ 0aC2 whereas the sample to start with was 12 % CaC2. They 
 also noted that NaCl, CaCl and iron powder aided in the de- 
 composition of the carbide. When CO gas is passed over CaC2 
 at temperatures between 200-250°C, there is a reaction talcing 
 place as indicated 
 
 GaC2 4 GO = CaO 4 3C 
 
 At 1600^0 this reaction is reversible. It may be well 
 to note here that according to this equation the carbide must 
 be formed at high temperatures. 
 
 Since my problem is one of a reducing nature, it may 
 
 / 
 
 be well to summarize the work that has been done along this 
 line. As early as 1899 we find Tarugi (2) worked on the re- 
 ducing properties of calcium carbide. He reduced copper 
 oxide at bright red heat and the chloride of copper at about 
 400°C. Ktigelgen (3) has done extensive work on the reducing 
 properties of calcium carbide. He worked with the oxides of 
 Pb, Cu, Ag, Zn, Hg, Sn, As, W, Mn, Fe, Ni, Al. 
 
 If a mixture as indicated by the equation below is 
 heated to dull red heat a reduction takes place as indicated; 
 
 (1) PbO 4 GaG2 = Pb 4 GaO 4 20 
 
 At dull red heat the carbon, which is the graphitic 
 form will react as indicated: 
 
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4 
 
 (2) 4PbO 4 2C = 4Pb 4 2CO2 
 
 If tile charge contains an excess of oxide it will re- 
 act according to equation (3) 
 
 (3) 5Pi>0 4 CaCg = 5Pb 4 CaO 4 2CO2 
 
 This reaction will take place at higher temperatures, 
 while 1 and 2 at lower temperatures. The chloride of Lead re- 
 acts in a similar manner. 
 
 (4) PhCl;> 4 CaC2 = Pb 4 CaCl2 4 2C 
 
 A mixture of the oxide and chloride react according to 
 
 (5) 
 
 (5) 4PbO 4 PbCl2 4 CaC2 = 5Pb 4 CaCl2 4 2CO2 
 
 These reactions may be considered as the general re- 
 actions of calcium carbide with oxide and chlorides of all of 
 the metals named previously. 
 
 FrohUch (4) showed that 1/10 to 1/4 ton of CaC2 was 
 necessary to produce 1 ton of copper. Kilgelgen worked with 
 the oxides of iron and CaC2. He was able to get a reduction, 
 but claims that it is of no definite value as in the case of 
 lead and copper. Prom what has been discussed so far we can 
 represent the reduction of oxides by carbides by two general 
 equations: 
 
 ( 1 ) 3M0 4 CaC2 = CaO 4 3M 4 2C0 
 
 (2) 5M0 4 CaC2 = CaO 4 5M 4 2CO2 
 
 The first takes place with oxides difficultly reduced 
 (according to Newmann and Frohlich) . The second with oxides 
 easily reduced (Kugelgen), 
 

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5 
 
 Calcium carbide has been used as a desulphurizing and 
 deoxidizing agent in the metallurgical Industry mainly in the 
 electric furnace where high temperatures are possible. T. M. 
 Camp and C. B. Francis in their book, "The Making Shaping and 
 Treating of Steel" give the following theory in regards to 
 the action and fomation of Calcium Carbide in the Heroult 
 Furnace, Under the influence of the high temperatures that 
 exist around the electrode the CaO and carbon in their vicin- 
 ity combine to form calcium carbide. The authors maintain 
 that it is at that point when desulphurization takes place. 
 The slags of the Heroult furnace contain various amounts of 
 free CaC 2 . The authors claim that a considerable quantity of 
 CaC 2 in the slag is a guarantee that the bath is deoxidized. 
 
 CaC2 4 
 
 3FeO 
 
 3MnO 
 
 3Fe 
 
 3Mn 
 
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 Moisson (5) did work on the reaction of sulfides with 
 calcium carbide. 
 
 FeS 4 CaC 2 = Fe 4 CaS 4 2C 
 From the above reactions one can see that CaCg in the 
 slag seiwes as a deoxidizer and desulphurizer. 
 

 
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6 
 
 EXPERIMENTAL 
 
 For my experimental work it was necessary to determine 
 accurately, the purity of the calcium carbide and iron oxide 
 used. The iron oxide was determined by the Permanganate 
 method. The CaCg was analyzed by two methods. 
 
 (1) Absorbtion in Wprous chloride. 
 
 (2) Difference in weight method. 
 
 These methods can be combined so that one is a check 
 for the other. The apparatus illustrated below was used. 
 
 A 
 
 A B D E G H 
 
 A contains H 2 SO 4 to dry air passing through apparatus. 
 B is the acetylene generator. 
 
 C a calcium chloride tube. 
 
 D a trap 
 
 E contains a hypochlorite colution for removing sulfur 
 and phosphorus. 
 
 P a calcium chloride tube. 
 

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7 
 
 Q- and H contain an ammonlacle solution of cuprous 
 chloride. 
 
 I is a CaCl 2 tube. 
 
 The cuprous chloride solution was prepared as given 
 in Bloxam. 
 
 30 grams of black copper oxide dissolved in 200 c.c. 
 of HGl and boiled for 30 minutes with 24 grams of finely di- 
 vided copper. The brown solution is poured into 1750 c.c. of 
 H20, allowed to settle, the water drawn off by a siphon and 
 the precipitate rinsed into a 1/2 liter bottle. This is 
 filled with water and when the ppt. is settled the water is 
 drawn off as before. 120 grams of NH 4 CI are added and the 
 bottle filled with water and shaken. For precipitation this 
 solution is poured into 1/10 its bulk of strong ammonia. 
 
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 dry flask B which is fitted with a dropping funnel and delivery 
 tubes as indicated. A sli^t excess over the calculated 
 amount of water is added. It is best to use a 20^ salt (NaCl) 
 solution as this will reduce the heating effect. B and C are 
 carefully v/eighed (to the third place), G-, H and I are also 
 weighed. The apparatus is connected to tightly fitting 
 rubber tubing. Stop cock o is opened slightly to allow a slow 
 stream of dry air to pass through the apparatus. The water 
 or salt solution is then allowed to drop very slowly. This 
 is necessary or else the gas will pass out unabsorbed. After 
 the reaction has stopped, the current of air is allowed to 
 
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pass through for about 2 hours in order to make sure that 
 all of the acetylene has passed into 0- and H. B and C and 
 G, H and I are again weighed. Since, according to the ti«o 
 equations, 
 
 (1) CaC^ 4 H 2 O = Ca(0H)2 4 
 
 (2) C 2 H 2 4 CuCl 4 2 NH 3 = Cu C C Cu 4 2 NH 4 CI 
 
 all of the products remain in the apparatus, the loss 
 in weight of B and C should equal the gain in weight of G, H 
 and I. The loss in weight of B and C equals the weight of 
 C 2 H 2 produced, corrected for weight of hydrogen sulfide and 
 phosphide evolved. The cuprous acetylide comes down as a red 
 precipitate which is insoluble in water. In the analysis, the 
 absorption method was omitted. The difference method is 
 fairly accurate as will be seen by the results obtained. 
 
 WEIGHT OF 
 CaCo 
 
 WEIGHT OF 
 APPARATUS 
 B4C before 
 
 WEIGHT OF 
 B 4 C 
 after 
 
 DIFFEREITCE 
 = Wt. of 
 C 2 H 2 
 
 ^PURE 
 
 CaC2 
 
 AVSRAGE 
 
 23.4837 
 
 372.697 
 
 368.450 
 
 4.247 
 
 44.57 
 
 
 7.0663 
 
 379.011 
 
 377.715 
 
 1.296 
 
 44.60 
 
 
 7.6758 
 
 304.470 
 
 302.987 
 
 1.483 
 
 47.29 
 
 
 7.7358 
 
 336.346 
 
 334.937 
 
 1 .409 
 
 44.80 
 
 45.31 
 
 
 Second Sample 
 
 
 
 
 5.3588 
 
 276.544 
 
 274.894 
 
 1.650 
 
 75.75 
 
 
 4.4914 
 
 229.132 
 
 227.698 
 
 1.434 
 
 78.60 
 
 
 5.1221 
 
 278.510 
 
 276.929 
 
 1 .581 
 
 76.02 
 
 76.79 
 
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9 
 
 The first sample used was very finely divided material 
 which had been exposed to the air. For this reason, the 
 sample is rather low in carbide. The second sample was coar- 
 sely ground and only large lusterous lumps of carbide were 
 ground. The iron oxide ran 88.6^ and 90% pure Fe^O^* Only 
 traces of S were found in either sample. 
 
 FUSIONS 
 
 In order to determine the reaction of Calcium Carbide 
 on iron oxide various charges and temperatures were tried. 
 
 The ultimate aim was to reach a temperature condition similar 
 to that in the open hearth furnace. For temperatures up to 
 1250^0 a gas furnace was used and above this temperature an 
 oil furnace was used. 
 
 Fusion No. I 
 A B 
 
 CaC 2 6.150 grams 5.673 grams 
 
 ^ 620 ^ 15.375 grams 14.182 grams 
 
 C 1 gram 1 gram 
 
 This charge is calculated according to the equation: 
 CaC 2 4 FegOj = 2Fe 4 CaO 4 2C0 
 All figures are based on chemically pure materials. 
 
 The two charges were heated for 3 hours at 1050 to 1100°C. 
 
 In both cases the charges were slightly fused, but did not 
 adhere to the crucibles. The fused charges were ground and 
 treated for undecomposed CaC 2 . The charge was placed in B. 
 Water was first added, then a dilute solution of HCl, but no 
 
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10 
 
 acetylene was detected in the cuprous chloride solution. 
 
 Two similar charges were then heated to 1200-1250^0 
 for three hours. At this temperature the charges were partly 
 fused and adhered to the crucible. On cooling, the upper part 
 of the charge contained a grey powder, which on analysis was 
 found to be iron. In this case undecomposed carbide was 
 analyzed for, but none was detected. The free iron in the 
 charge could not be determined as there was present with it 
 unreacted Fe^O^ and perhaps other iron compounds as well. 
 
 In the next ffiisions the charges were made up according 
 to this equation. 
 
 5 Fe 203 4 3 CaC 2 = lOFe + 3Ca0 1 6 CO 2 
 Charpies C D E F 
 
 CaC 2 5.520 5.438 5.330 5.401 
 
 Fc203 25.850 25.31 25.00 25.23 
 
 12 grams of slag material of the composition given 
 below were added to charges E and F. 
 
 AI 2 O 3 - 3 grams 
 
 CaCO^ - 5 grams 
 
 NagCO^ - 5 grams 
 
 CaF - 5 grams 
 
 Si 02 - 12 grams 
 
 These charges were heated to white heat, approximately 
 1400°C, for two hours. No attempt was made to pour these 
 charges. When removed from the fximace the charges were 
 fluid. A glass like slag was produced in all four charges. 
 

 
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11 
 
 Charge C contained a small head of Iron at the bottom weigh- 
 ing .2068 grams. Charge E contained a bead weighing 1.253 
 grams. No carbide was detected on analysis. From the above 
 results it showed that most of the ^^ 2 ^^ went into the slag. 
 The addition of slag material produced a larger button. If 
 we assume 1.253 grams, the weight of all the iron reduced in 
 charge E, then only 1.789 grams of FegO^ was reduced by the 
 carbide. This is a reduction of 7.15^ 
 
 The next charges contained the calculated amount of 
 ^®2*^3 an excess approximately equivalent to the amount 
 
 that went into the slag in charges C, D, E and F, The new 
 charges were given the same heating and then poured in an iron 
 mold, G-raphlte crucibles were used here instead of the clay 
 crucibles. 
 
 RESULTS 
 
 Charges 
 
 a 
 
 H 
 
 I 
 
 CaC 2 used 
 
 6.27 
 
 6.4 
 
 7.27 
 
 Fe 20 - used 
 
 50 
 
 50 
 
 60 
 
 Wt. of Fe 
 
 14.34 
 
 26.76 
 
 21.03 
 
 % Reduction 
 
 28.7 
 
 53.5 
 
 35.00 
 
 The above table gives the results obtained in the last 
 fusion. The slag in each case could be partly poured. In 
 no case was the iron button larger than about 4 grams. The 
 slag contained much of the free iron in the form of small 
 beads. The slag was broken up to remove the beads of iron. 
 
 A strong magnet was used to separate the iron from the slag. 
 

 
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12 
 
 This was added to the iron buttons. Under the conditions of 
 the charge and the temperature to which it was heated it is 
 not probable that any of the iron that was removed by the 
 magnet was magnetite. Any Pe^O^ formed could react according 
 to the equation below. 
 
 4 0 = 3FeO 4 00 
 
 This reaction takes place at 1175°C. The temperature 
 of the fusion was about 1400^^0. From this I conclude that 
 there was little or no magnetite formed in the charge. 
 
 Before dissolving the iron a microscopic examination 
 was made of the iron buttons of charges H and I. 
 
 The microphotographs are characteristic of medium 
 carbon steel, approximately 45 carbon. The difference in 
 structure is due to a change in the rate of cooling. 
 

 
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13 
 
 CONCLUSIONS 
 
 (1) The results clearly show that when calcium carbide is 
 heated in the presence of Pe^Oj at 1000*^ a slight reducing 
 action takes place* The reaction increases as the tempera- 
 ture is increased. Note last results. 
 
 (2) Since no acetylene could be detected when the fused 
 charges were treated with water and dilute HCl it seems that 
 the carbide is not present as CaC^* but in some form unde- 
 termined. 
 
 (3) At temperatures of 1400° and above there is a distinct 
 reduction as shown in the data. 
 
 (4) The iron produced is of medium carbon content. Approx- 
 imately 0.45^. 
 
 (5) The fluidity of the slag seems to have an apparant e 
 effect on the separation of the reduced iron. 
 
 (6) The results clearly show that when CaC2 is added to 
 remove sulphur from steel it also reacts as a deoxidizing 
 agent when oxides are present. Whether or not calcium carbide 
 is of any commercial value as a reducing agent the writer 
 cannot say. The results indicate that there is a distinct 
 reaction taking place at or neat temperatures maintained in 
 
 an open hearth furnace. 
 

 
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14 
 
 Note: - This thesis represents one semesters work. Had 
 
 more time been devoted, many more results would have 
 been obtained and perhaps a much better understanding 
 and explanation of the problem. 
 
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BIBLIOGRAPHY 
 
 1. Z. Elect. 
 
 2. Gazetta 
 
 3. Z. E. 
 
 4. Zeitssh. f 
 
 5* J. 0. C. 
 
 -17 - 177 - 9 
 
 1899 29: 509-512 
 
 1901 -7- 541-550 
 
 557-568 
 573-580 
 
 , Ansuvchem 1899 - 1179 
 
 1898 Ail 333 
 

 '4A''-' 
 
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