Historic, archived document Do not assume content reflects current scientific knowledge, policies, or practices Iss"ed January tt o x-^-r^ 19, ]0! o. U. S. DEPARTMENT OF AGRICULTURE, BUREAU OF CHEMISTRY-BULLETIN No. 130. H. W. WILEY, Chief of Bureau. MANUFACTURE OF DENATURED ALCOHOL. of m e™imeNtal STILLZmTS?"AT WASHINGTON, D. C. AND A COCINF of LECTURES DELIVERED IN CONNECTION THEREWITH By H. W. WILEY, Chief, Bureau of Chemistry, WITH THE COLLABORATION OF H. E. SAWYER, L. M. TOLMAN, A. H. BRYAN, A. GIVEN and H. W. BERGER. WASHINGTON: GOVERNMENT PRINTING OFFICE, 1910. LETTER OF TRANSMITTAL. U. S. Department of Agriculture, Bureau of Chemistry, Washington, D. C, August 7, 1909. Sir: I submit herewith the manuscript reporting the proceedings of the school established by you for teaching the principles of indus- trial distillation, and also the results obtained by the operation of the experimental industrial distillery erected in harmony with your direc- tions for the purpose of making industrial alcohol, especially from farm and factory wastes. One of the principal objects of this instruc- ! tion and of these experiments was to teach young men connected with the agricultural colleges and experiment stations the theory and practice of industrial distillation. To this end the distillery was i operated in connection with the school of instruction, and various waste materials such as could be found upon the farm, and also the refuse of factories using agricultural products, were employed as raw i materials. One of the most useful results of an experimental work of ! this kind is to ascertain the principal difficulties which stand in the i- way of a successful establishment of agricultural distillation for industrial purposes, and until these difficulties are thoroughly under- stood and methods for removing them are established it is not reason- able to expect the development of an agricultural distilling industry in this country. Although now almost three years have elapsed since the passage of the act permitting the use of industrial alcohol free of tax, not a single agricultural distillery has yet been successfully established. It is believed, however, that the information which is contained in the manuscript submitted will be extremely useful in promoting the cause of industrial distillation, especially among agri- cultural communities. I recommend that it be published as Bulletin No. 130 of the Bureau of Chemistry. Respectfully, H. W. Wiley, Chief of Bureau. Hon. James Wilson, Secretary of Agriculture. CONTENTS. Page. Introduction 9 Alcohols and alcoholometry 11 Chemical composition of alcohols 11 Methyl alcohol 12 Ethyl alcohol 13 Higher alcohols 14 Aldehydes, acids, and esters 14 Alcoholometry 15 Sources of alcohol 18 Chemistry of the carbohydrates 18 True sugars 18 ___^-Starch 21 Dextrin 22 Cellulose 23 Inulin, levulin, and other substances 23 Raw materials 24 Saccharine materials 25 Starchy materials 30 Fermentation processes 32 Classification of enzyms and their action 32 Carbohydrate enzyms 32 Proteolytic enzyms 34 Zymase 34 Oxydases 35 Lipases 36 Malting. By J. A. Le Clerc 36 Types of malting barleys and their composition 36 Physical characteristics 37 Malting operations 38 Green malt . 40 Composition of malt and the accompanying changes in the barley 41 Preparation of material for fermentation 42 Saccharine materials 42 Mashing of starchy materials 43 The open mash tub 44 Vacuum cooker 45 Henze cooker and mash tub for potatoes. 46 The yeast and its preparation 48 Kind of yeast 49 Raw material for the yeast mash and its saccharification 49 Souring of the yeast mash 50 Fermenting the yeast 51 Development of the start yeast. 51 Potato yeast 52 5 1 6 DENATURED ALCOHOL. Page. Distillation 53 Operation of a small laboratory still 53 The thermology of distillation 54 The earliest type of industrial still (fire pot still) 57 Operation 58 Causes of unusual expense 60 i Operation of an experimental distillery for making industrial alcohol 62 Purposes and capacity of the distillery 62 Equipment of the experimental distillery 63 Course of a mash through the distillery 64 1 Experimental runs using low-grade materials 66 Physical and chemical tests in the distillery 70 Simple tests 70 Saccharimetric determinations 70 Completeness of saccharification of the mash 71] Acidity determinations 71 Diastase in the fermented mash 72 Moisture in grain and malts 72] Analytical determinations 73 Diastasic power of malt Tc l Starch and sugar in raw materials 7 . Protein in raw material and slop 74 Ungelatinized starch in the mash 74 Fermentable substances in the fermented mash 74 Alcohol in the fermented mash and slop 75 Denatured alcohol and denaturants. By C. A. Crampton 76 Discussion of term "denatured alcohol " 76 Denaturing systems and formulas of different nations 77 Denaturing formulas adopted by the United States 80 Special denaturants ?7T^^ . ^. 81 Conclusion 84 Miscellaneous lectures 85 Programme for course on denatured alcohol 85 Purposes and scope of proposed course on fermentology. By H. W. Wiley 86 The history of distillation. By H. W. Wiley 90 Sources of alcohol 94 Utilization of cereals in the manufacture of denatured alcohol. By H. W. Wiley 94 Utilization of potatoes in the manufacture of denatured alcohol. By H. W. Wiley 97 Cassava and sweet potatoes as sources of industrial alcohol. By C. C. Moore 99 The possibilities of bananas for making industrial alcohol. By G. N. Collins 104 Alcohol from cactus. By W. W. Skinner 105 Prickly pear and its fruits as a source of alcohol. By R. F. Hare 107 Distillery operation and control 109 Distillery practice. By J. A. Wathen 109 Yeasting. By J. A. Wathen , 113 Chemical control of distillery operations applying especially to grain distilleries. By A. M. Breckler 117 . CONTENTS. 7 Miscellaneous lectures—Continued. Page. Distillery operation and control—Continued. Practical yeasting of distilleries, with special reference to grain dis- tilleries. By A. M. Breckler 122 Practical operation of a distillery. By R. P. O'Brien 125 Effect of distillation in different types of stills. By L. M. Tolman 127 Bacteriological technique. By Geo. W. Stiles 133 Microscopical examinations. By B. J. Howard 136 Some special uses of industrial alcohol 138 Use of alcohol in varnish making. By F. P. Veitch 138 Use of alcohol for power. By R. M. Strong 141 Legislation and regulations 146 Legislation providing for the use of industrial alcohol. By John G. Capers 146 Regulations relating to industrial distilleries. By Wales Hubbard 152 Closing remarks on the denatured alcohol course. By H. W. Wiley 157 Appendix 159 Internal Revenue Circular No. 721, relating to the establishment and opera- tion of stills at agricultural experiment stations for the manufacture of denatured alcohol 159 Special denaturants 161 Statistics of denatured alcohol production 165 LLUSTRATIONS. Paga Fig. 1. Open mash tub 44 2. American vacuum cooker 46 3. Henze cooker and German mash tub 47 4. Small laboratory still 53 5. Fire pot still 58 6. Modified copper pot still, showing doubler and connections 61 7. American types of distilling apparatus 62 8. Floor plan, experimental distillery 64 9. Side elevation, experimental distillery 65 10. Continuous column still, experimental distillery 66 11 End view of apparatus for moisture determination in grain 73 12. Early stills in the shapes of animals 91 13. Some ancient forms of stills 92 14. Fractionation in a pot still 129 15. Comparison of proof of distillate and temperature in column and in pot stills 130 MANUFACTURE OF DENATURED ALCOHOL. INTRODUCTION. Since June 7, 1906, a statute of the United States has provided that domestic alcohol may be withdrawn from bond without the payment of an internal-revenue tax, for use in the arts and indus- tries, and for fuel, light, and power, on condition that it shall have been denatured by the admixture of some material which unfits it for use medicinally or as a beverage. The main purpose of this act, known commonly as the "Denatured Alcohol Law," was to reduce the cost of alcohol to the industrial consumer, and it was believed that this end would be attained, not only by the remission of the tax, but in many cases by the special manufacture of industrial alcohol from cheaper materials than have been utilized in the past in making potable alcohol. It became apparent, however, that such materials—like farm waste of different sorts—are most abundant in farming communities remote from the existing centers of the distil- ling industry and that it would be necessary in securing their utiliza- tion to encourage the establishment of small farm distilleries in neighborhoods where such waste is abundantly available. There- fore, in 1907, it was provided, by an amendment to the original act, that special encouragement might be given by the Commissioner of Internal Revenue to distilleries producing industrial alcohol in amounts less than 100 proof gallons daily by the removal of many of the restrictions which are imposed on larger distilleries and on those in which potable alcohol is produced. It was believed that as a result of this action it would be possible for farmers to make crude alcohol at so low a cost that they could utilize it advantageously upon their farms as a source of power, light, and heat; and it was expected that many communities would establish such agricultural distilleries as were contemplated by the act. Over a year passed, however, without any attempts to make alcohol upon this plan, to the serious disappointment of all who were interested in the matter, and it became apparent that further official encouragement was needed. By numerous misleading publications a great many people had been led to believe that any waste vegetable material, though of the most worthless character, can profitably be used in making alcohol. 9 K) DENATURED ALCOHOL.