metafractal
January 12th, 2003, 12:22 PM
While looking through some old books, I came across an old, falling appart, pamphlet: "Instructions for the Manafacture of Saltpetre by Joseph Leconte ... South Carolina 1862". Upon reading, it was an in depth guide of how any farmer can prepare a nitre-bed out of various plant and animal matter. I soon realized that it was written at the time of the American civil war...
The core of the information is as follows:
"...The general conditions necessary to the formation of saltpetre are: 1st, the presence of decaying orgainic matter, animal or vegetable, especially the former; 2nd, an alkaline or earthy base, as potash or lime; 3rd, sufficient moisture; 4th, free exposure to the oxygen of the air; and 5th, shelter from sun or rain.
These conditions are found in nature, as in the soil of all caves, but particularly of those in limestone countries; and still more frequently under a concurrence of circumstances ... cellars, manure heaps, stables ... dirty streets and lanes."
Then it goes on to explain the process of nitrification, which I see no need to post here, and rants on about how the confedoracy needs you to do this to keep you freedom, but we're all full hearted confederates already, so no need for this :D .
Finally, it goes into depth about the preparation of the beds:
"The most important prerequisite in the construction of nitre-beds in such manner as to yield nitre in the shortest possible time is a good supply of thoroughly rotted manure of the richest kind, in the condition usually called Mould or Black Earth"
"... to make the bed a floor is prepared of clay, old mortar coarsley ground, or wood ashed (leached ashes will do), together with leaves, straw, small twigs, branches, to give porosity to the mas, and a considerable quantity of common earth, if this has not been added to the original manure-heap. The mixture is thrown somewhat lightly on clay floor, so as to form a porous heap four or five feet high, six or seven wide, and fifteen feet long. The whole is then covered by a rough shed to protect from weather, and perhaps protected on the sides in some degree from winds. The heap is watered every week with the richest quantity of liquid manure, such as urine dung-water, warter of privies (?), cess-pools, drains, etc. The quantity of liquid should be such as to keep the heap always moist, but never wet. Drains, also, may be constructed as to conduct any superfluous liquid to a tank, where it is preserved and used in watering heaps. The materials are turned over to a depth of five or six inches every week, and the whole heap turned over every month. This is not always done, but it largeley hastens the process of nitrification. During the last few months of the process, no more urine, nor liquid manure of any kind, must be used, but the heaps must be kept moist by water only. The reason for this is that undecomposed organic matter interferes with the separation of the nitre from the ley. As the heap ripens, the nitre is bought to the surface by evabouration, and appears as a whitish efflorescence, depth of two or three inches, and put aside under shelter, and kept moist with water. The nitre cointained is considerable increased. When the whitish crust appears, it is again removed until a quantity sufficient for leaching is obtained. The small mound which is thus left is usually used as the nucleus of a new heap. By this method it is believed that an abundant supply of nitrified earth, in a condition fit for leaching, may be obtained by autumn or early winter NB: this meant about ten months from the time of writing".
It then goes into depth about mass production and foreign methods of the preparation of nitre beds, but such is beyond the scope of this post. Fact: at that time, the Swedes payed a portion of their taxes in nitre compounds! My how times have changed :p .
Finally, it describes the method of leaching, crystalization, purification, and Analisys.
"Leaching. When the process of nitrification is complete, the earth of the heaps must be leached. Manufacturers are accustomed to judge roughly of the amount of nitre in any earth by the taste. A more accurate method is by leaching a small quantity of the earth, and boiling to dryness, and weighing the salt. There is much diversity of opinion as to the per centage of nitre necessary to render its extraction profitable. The best writers on this subject vary in their estimates from fifteen pounds to sixty pounds of salt per cubic yard of nitrified earth. The high price of nitre with us at present would make a smaller per centage profitable. This point, however, will soon be determined by the enterprising manufacturer.
In the process of leaching, in order to save fuel, we must strive to get as strong a solution as possible, and at the same time to extract all or nearly all the nitre. These two objects can only be attained by repeated leachings of the same earth, the ley thus obtained being used on fresh earth until the strength of the ley is sufficient. A quantity of nitrified earth is thrown into a vat, or ash-tub, or barrel, or hogshead with an aperture below, closely stopped and covered lightly with straw. Water is added, about half as much in volume as the earth. After stirring, this is allowed to remain twelve hours. Upon opening the bung, about half the water runs through containing, of course, one-half the nitre. Pure water, in quantity half as much as first used, is again poured on, and after a few moments run through. This will contain one-half the remaining nitre, and therefore one-fourth of the original quantity. Thus the leys of successive leachings become weaker and weaker, until, after the sixth leaching, the earth is considered as sufficiently exhausted. The exhausted earth is thrown back on the nitre-beds, or else mixed with black earth to form new beds. The leys thus obtained are used upon fresh earth until the solution is of sufficient density to bear an egg. It then contains about a pound of salt to a gallon of liquid.
Conversion.The ley thus obtained contains, besides nitrate of potash (nitre), also nitrate of lime and magnesia, and chlorides of sodium and potassium. The object of the next process is to convert all other nitrates into nitrate of potash. This is done by adding wood ashes. The potash of the ashes takes all the nitric acid of the other nitrates forming the nitrate of potash (nitre), and the lime and magnesia are precipitated as an insoluble sediment. Sometimes the ashes is mixed with the nitrified earth and leached together, sometimes the saltpetre ley is filtered through wood ashes, sometimes the ley of ashes is added to the saltpetre ley. In either case the result is precisely the same." NB: depending on the use for the nitrates, one may wish to omit this step, save some of the MgNO3, or a magnitude of other things.
"Crystalization The ley thus converted is then poured off from the precipitate, into copper or iron boilers. It still contains common salt (chloride of sodium) in considerable, and some other impurities in smaller, quantities. It is a peculiarity of nitre, that it is much more soluble than common salt in boiling water, but much less soluble in cold water. As the boiling proceeds, therefore, and the solution becomes more concentrated, the common salt is, most of it, precipitated in small crystals, as a sandy sediment, and may be raked out. Much organic matter rises as scum, and must also be removed. When the concentration has reached almost the point of saturation, the boiler must be allowed to cool. This is known by letting fall a drop of the boiling liquid upon a cold metallic surface; if it quickly crystallizes, it is time to stop the boiling. It is now poured into large receivers and left to cool. As the ley cools, nearly the whole of the nitre separates in the form of crystals, which sink to the bottom. These are then removed, drained by throwing them in baskets, and dried by gentle beat. The mother-liquor is either thrown back into the boilers, or else used in watering the heaps. The product thus obtained is the crude saltpetre of commerce. It still contains fifteen to twenty-five per cent. of impurities, principally common salt (chloride of sodium), chloride of potassium and organic matter.
Refining . One hundred gallons of water is poured into a boiler, and crude saltpetre added from time to time, while the liquid is heating, until four thousand pounds are introduced. This will make a saturated solution of nitre. The
scum brought up by toiling must be removed, and the undissolved common salt scraped out. About sixty gallons cold water is now added gradually, so as not to cool the liquid too suddenly. From one to one and a-half pounds of glue, dissolved in hot water, is added, with stirring. Blood is sometimes used instead of glue. The glue seizes upon the organic matter, and they rise together as scum, which is removed. Continue the boiling until the liquid is clear. The liquid is then suffered to cool to one hundred and ninety-four degrees, and then carefully ladled out into the crystallizers. These are large shallow vats, with the bottom sloping gently to the middle. In these the cooling is completed, with constant stirring. In the process of cooling nearly the whole of the nitre is deposited in very fine, needle-like crystals, which, as they deposit, are removed and drained. In this condition it is called saltpetre flour. The object of the constant stirring is to prevent the aggregation of the crystals into masses, from which it is difficult to remove the adhering mother-liquor. The saltpetre flour is then washed of all adhering mother-liquor. For this purpose it is thrown into a box with a double bottom; the lower bottom with an aperture closely plugged, and the false bottom finely perforated. By means of a watering pot a saturated solution of pure nitre is added, in quantity sufficient to moisten thoroughly the whole mass. After remaining two or three hours to drain, the plug is removed and the solution run out. This is sometimes repeated several times. The saturated solution of nitre cannot, of course, dissolve any more nitre, but dissolves freely the impurities present in the adhering mother-liquor. Last of all, a small quantity of pure water-- only about one pound to fifty-three pounds of the nitre to be washed-- is added in the same manner, and run off at the end of two hours. The nitre is now dried by gentle heat and constant stirring, and may be considered quite pure, and fit for the manufacture of gunpowder."
Phew. Thats was a lot of typing. In retrospect OCR would have been a better choice :D (still, I dont see it working too well with that battered old thing...)
It should be kept in mind that this was written for the deep southern American climate. This is not dissimilar to that of outback Australia, where many of our members do live.
The method could be improved in numerous ways with todays knowledge of chemistry. Markedly, the addition of nitrifying bacterior would speed the process up dramatically. I have seen such bacterior sold at hydroponics stores. Is there any limit (within reason) to the amount of nitrifying bacterior that could be added? The times may become relativeley fast if such is done. I would also further control the conditions of the bed to optimize them. The methods of refinement, leaching, etc could obviously be improved with today's common lab equipment and procedures and need little discussion here. Input on the improvement of the beds would be appreciated.
The method is only applicable at all to those living in open, rural areas. While it seems a rather tedious and unproductive way of doing so, it has an huge obvious advantage: untracable sources = no suspicion. I am paranoid, and I like to keep my slate 100% clean. No one has ever suspected anything no matter what I buy. I like it that way. It is really only imperative when scaling a 'major operation' (i.e. when large amounts of nitrates need to be acquired cheaply and without suspicion.) The foremost problem with HNO3 from xNO3/H2SO4 is the unwillingness to waste nitrates...
The information may become more valuable when KNO3 dries up worlwide (which I'm sure it will, as has been mentioned in a separate post, in the 60s you could buy TNT from many rural hardware stores...)
I will sureley build one right next to my lab (i.e. hut/shed I built out of scrap wood and metal in a dried up riverbed :D ). I do so more as a scientific inquiry than a viable source of nitrates (while I'm not complaining about the KNO3 <img border="0" title="" alt="[Wink]" src="wink.gif" /> ). I will tell you all how it goes, along with the improvements I make to this method.
The core of the information is as follows:
"...The general conditions necessary to the formation of saltpetre are: 1st, the presence of decaying orgainic matter, animal or vegetable, especially the former; 2nd, an alkaline or earthy base, as potash or lime; 3rd, sufficient moisture; 4th, free exposure to the oxygen of the air; and 5th, shelter from sun or rain.
These conditions are found in nature, as in the soil of all caves, but particularly of those in limestone countries; and still more frequently under a concurrence of circumstances ... cellars, manure heaps, stables ... dirty streets and lanes."
Then it goes on to explain the process of nitrification, which I see no need to post here, and rants on about how the confedoracy needs you to do this to keep you freedom, but we're all full hearted confederates already, so no need for this :D .
Finally, it goes into depth about the preparation of the beds:
"The most important prerequisite in the construction of nitre-beds in such manner as to yield nitre in the shortest possible time is a good supply of thoroughly rotted manure of the richest kind, in the condition usually called Mould or Black Earth"
"... to make the bed a floor is prepared of clay, old mortar coarsley ground, or wood ashed (leached ashes will do), together with leaves, straw, small twigs, branches, to give porosity to the mas, and a considerable quantity of common earth, if this has not been added to the original manure-heap. The mixture is thrown somewhat lightly on clay floor, so as to form a porous heap four or five feet high, six or seven wide, and fifteen feet long. The whole is then covered by a rough shed to protect from weather, and perhaps protected on the sides in some degree from winds. The heap is watered every week with the richest quantity of liquid manure, such as urine dung-water, warter of privies (?), cess-pools, drains, etc. The quantity of liquid should be such as to keep the heap always moist, but never wet. Drains, also, may be constructed as to conduct any superfluous liquid to a tank, where it is preserved and used in watering heaps. The materials are turned over to a depth of five or six inches every week, and the whole heap turned over every month. This is not always done, but it largeley hastens the process of nitrification. During the last few months of the process, no more urine, nor liquid manure of any kind, must be used, but the heaps must be kept moist by water only. The reason for this is that undecomposed organic matter interferes with the separation of the nitre from the ley. As the heap ripens, the nitre is bought to the surface by evabouration, and appears as a whitish efflorescence, depth of two or three inches, and put aside under shelter, and kept moist with water. The nitre cointained is considerable increased. When the whitish crust appears, it is again removed until a quantity sufficient for leaching is obtained. The small mound which is thus left is usually used as the nucleus of a new heap. By this method it is believed that an abundant supply of nitrified earth, in a condition fit for leaching, may be obtained by autumn or early winter NB: this meant about ten months from the time of writing".
It then goes into depth about mass production and foreign methods of the preparation of nitre beds, but such is beyond the scope of this post. Fact: at that time, the Swedes payed a portion of their taxes in nitre compounds! My how times have changed :p .
Finally, it describes the method of leaching, crystalization, purification, and Analisys.
"Leaching. When the process of nitrification is complete, the earth of the heaps must be leached. Manufacturers are accustomed to judge roughly of the amount of nitre in any earth by the taste. A more accurate method is by leaching a small quantity of the earth, and boiling to dryness, and weighing the salt. There is much diversity of opinion as to the per centage of nitre necessary to render its extraction profitable. The best writers on this subject vary in their estimates from fifteen pounds to sixty pounds of salt per cubic yard of nitrified earth. The high price of nitre with us at present would make a smaller per centage profitable. This point, however, will soon be determined by the enterprising manufacturer.
In the process of leaching, in order to save fuel, we must strive to get as strong a solution as possible, and at the same time to extract all or nearly all the nitre. These two objects can only be attained by repeated leachings of the same earth, the ley thus obtained being used on fresh earth until the strength of the ley is sufficient. A quantity of nitrified earth is thrown into a vat, or ash-tub, or barrel, or hogshead with an aperture below, closely stopped and covered lightly with straw. Water is added, about half as much in volume as the earth. After stirring, this is allowed to remain twelve hours. Upon opening the bung, about half the water runs through containing, of course, one-half the nitre. Pure water, in quantity half as much as first used, is again poured on, and after a few moments run through. This will contain one-half the remaining nitre, and therefore one-fourth of the original quantity. Thus the leys of successive leachings become weaker and weaker, until, after the sixth leaching, the earth is considered as sufficiently exhausted. The exhausted earth is thrown back on the nitre-beds, or else mixed with black earth to form new beds. The leys thus obtained are used upon fresh earth until the solution is of sufficient density to bear an egg. It then contains about a pound of salt to a gallon of liquid.
Conversion.The ley thus obtained contains, besides nitrate of potash (nitre), also nitrate of lime and magnesia, and chlorides of sodium and potassium. The object of the next process is to convert all other nitrates into nitrate of potash. This is done by adding wood ashes. The potash of the ashes takes all the nitric acid of the other nitrates forming the nitrate of potash (nitre), and the lime and magnesia are precipitated as an insoluble sediment. Sometimes the ashes is mixed with the nitrified earth and leached together, sometimes the saltpetre ley is filtered through wood ashes, sometimes the ley of ashes is added to the saltpetre ley. In either case the result is precisely the same." NB: depending on the use for the nitrates, one may wish to omit this step, save some of the MgNO3, or a magnitude of other things.
"Crystalization The ley thus converted is then poured off from the precipitate, into copper or iron boilers. It still contains common salt (chloride of sodium) in considerable, and some other impurities in smaller, quantities. It is a peculiarity of nitre, that it is much more soluble than common salt in boiling water, but much less soluble in cold water. As the boiling proceeds, therefore, and the solution becomes more concentrated, the common salt is, most of it, precipitated in small crystals, as a sandy sediment, and may be raked out. Much organic matter rises as scum, and must also be removed. When the concentration has reached almost the point of saturation, the boiler must be allowed to cool. This is known by letting fall a drop of the boiling liquid upon a cold metallic surface; if it quickly crystallizes, it is time to stop the boiling. It is now poured into large receivers and left to cool. As the ley cools, nearly the whole of the nitre separates in the form of crystals, which sink to the bottom. These are then removed, drained by throwing them in baskets, and dried by gentle beat. The mother-liquor is either thrown back into the boilers, or else used in watering the heaps. The product thus obtained is the crude saltpetre of commerce. It still contains fifteen to twenty-five per cent. of impurities, principally common salt (chloride of sodium), chloride of potassium and organic matter.
Refining . One hundred gallons of water is poured into a boiler, and crude saltpetre added from time to time, while the liquid is heating, until four thousand pounds are introduced. This will make a saturated solution of nitre. The
scum brought up by toiling must be removed, and the undissolved common salt scraped out. About sixty gallons cold water is now added gradually, so as not to cool the liquid too suddenly. From one to one and a-half pounds of glue, dissolved in hot water, is added, with stirring. Blood is sometimes used instead of glue. The glue seizes upon the organic matter, and they rise together as scum, which is removed. Continue the boiling until the liquid is clear. The liquid is then suffered to cool to one hundred and ninety-four degrees, and then carefully ladled out into the crystallizers. These are large shallow vats, with the bottom sloping gently to the middle. In these the cooling is completed, with constant stirring. In the process of cooling nearly the whole of the nitre is deposited in very fine, needle-like crystals, which, as they deposit, are removed and drained. In this condition it is called saltpetre flour. The object of the constant stirring is to prevent the aggregation of the crystals into masses, from which it is difficult to remove the adhering mother-liquor. The saltpetre flour is then washed of all adhering mother-liquor. For this purpose it is thrown into a box with a double bottom; the lower bottom with an aperture closely plugged, and the false bottom finely perforated. By means of a watering pot a saturated solution of pure nitre is added, in quantity sufficient to moisten thoroughly the whole mass. After remaining two or three hours to drain, the plug is removed and the solution run out. This is sometimes repeated several times. The saturated solution of nitre cannot, of course, dissolve any more nitre, but dissolves freely the impurities present in the adhering mother-liquor. Last of all, a small quantity of pure water-- only about one pound to fifty-three pounds of the nitre to be washed-- is added in the same manner, and run off at the end of two hours. The nitre is now dried by gentle heat and constant stirring, and may be considered quite pure, and fit for the manufacture of gunpowder."
Phew. Thats was a lot of typing. In retrospect OCR would have been a better choice :D (still, I dont see it working too well with that battered old thing...)
It should be kept in mind that this was written for the deep southern American climate. This is not dissimilar to that of outback Australia, where many of our members do live.
The method could be improved in numerous ways with todays knowledge of chemistry. Markedly, the addition of nitrifying bacterior would speed the process up dramatically. I have seen such bacterior sold at hydroponics stores. Is there any limit (within reason) to the amount of nitrifying bacterior that could be added? The times may become relativeley fast if such is done. I would also further control the conditions of the bed to optimize them. The methods of refinement, leaching, etc could obviously be improved with today's common lab equipment and procedures and need little discussion here. Input on the improvement of the beds would be appreciated.
The method is only applicable at all to those living in open, rural areas. While it seems a rather tedious and unproductive way of doing so, it has an huge obvious advantage: untracable sources = no suspicion. I am paranoid, and I like to keep my slate 100% clean. No one has ever suspected anything no matter what I buy. I like it that way. It is really only imperative when scaling a 'major operation' (i.e. when large amounts of nitrates need to be acquired cheaply and without suspicion.) The foremost problem with HNO3 from xNO3/H2SO4 is the unwillingness to waste nitrates...
The information may become more valuable when KNO3 dries up worlwide (which I'm sure it will, as has been mentioned in a separate post, in the 60s you could buy TNT from many rural hardware stores...)
I will sureley build one right next to my lab (i.e. hut/shed I built out of scrap wood and metal in a dried up riverbed :D ). I do so more as a scientific inquiry than a viable source of nitrates (while I'm not complaining about the KNO3 <img border="0" title="" alt="[Wink]" src="wink.gif" /> ). I will tell you all how it goes, along with the improvements I make to this method.